effect of loi of fly ash on properties of...
TRANSCRIPT
EFFECT OF LOI OF FLY ASH ON PROPERTIES
OF CONCRETE
BY
YOUPHALAT PHETHANY
A THESIS SUBMITTED IN PARTIAL FULFILLMENT OF THE
REQUIREMENTS FOR THE DEGREE OF MASTER OF SCIENCE
(ENGINEERING AND TECHNOLOGY)
SIRINDHORN INTERNATIONAL INSTITUTE OF TECHNOLOGY
THAMMASAT UNIVERSITY
ACADEMIC YEAR 2017
Ref. code: 25605722040416SAT
EFFECT OF LOI OF FLY ASH ON PROPERTIES
OF CONCRETE
BY
YOUPHALAT PHETHANY
A THESIS SUBMITTED IN PARTIAL FULFILLMENT OF THE
REQUIREMENTS FOR THE DEGREE OF MASTER OF SCIENCE
(ENGINEERING AND TECHNOLOGY)
SIRINDHORN INTERNATIONAL INSTITUTE OF TECHNOLOGY
THAMMASAT UNIVERSITY
ACADEMIC YEAR 2017
Ref. code: 25605722040416SAT
ii
Acknowledgements
The author would like to express his deepest gratitude to his advisor Dr.
Parnthep Julnipitawong for his continuously invaluable guidance and advice through
the duration of this thesis.
Sincere gratitude is also extended to his thesis committee members Prof. Dr.
Somnuk Tangtermsirikul, Dr Krittiya Kaewmanee for their valuable comments and
guidance on my thesis. A special thank is conveyed to Asst. Prof Dr Pitisan Krammart
of Rajamangala University of Technology Thanyaburi for serving as an external
examiner for this thesis. Another special thank is conveyed to Asst. Prof. Dr
Warakana Saengsoy and Dr. Lalita Yongchaitrakul for their memorable and valuable
advice.
Grateful acknowledgements are conveyed to AUN-seednet and Sirindhorn
International Institute of Technology (SIIT) for providing him the scholarship for
master degree at Sirindhorn International Institute of Technology, Thammasat
University.
The author also wishes to show his gratitude to his colleagues, senior project
students and laboratory technician for their assistance, support, advice and humor
during the laboratory and hismaster student life.
Special thanks are given to all staff of Sirindhorn International Institute of
Technology for their kind services and information throughout his study.
Finally and most importantly, he sincerely and gratefully dedicates this work
to his beloved family for their tremendous encouragement and constant support to his
study and all his life. He specially wants to thank his parents for their incomparable
love, sacrifices and patience.
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Abstract
EFFECT OF LOI OF FLY ASH ON PROPERTIES OF CONCRETE
by
YOUPHALAT PHETHANY
Bachelor of Engineering (Civil Engineering), National University of Laos, Laos, 2014
Master of Science (Engineering and Technology), Sirindhorn International Institute of
Technology, Thammasat University, Thailand, 2018
The quantity of low LOI fly ash available is decreasing worldwide as an
indirect result of controlling toxic gases such as nitrogen oxides (NOx) to meet the
emission standards of the 1990 Clean Air Act amendments. More recent coal power
plants around the world are equipped with low NOx burners in their boilers, which are
operated at lower firing temperature. This approach has an adverse effect on the
quality of fly ash produced because it increases the %LOI of the produced fly ash.
The term LOI basically stands for Loss on Ignition. Generally, the amount of
unburned carbon of fly ash can be easily determined by the LOI test (ASTM D7348).
High LOI fly ash is generally known to cause some malfunctions in concrete, which
are probably known to include discoloration, poor air entrainment ability, high water
requirement and low compressive strength. Therefore it was only utilized in low-
value method or disposed at landfills. So, to utilize these high LOI fly ashes in the
concrete work, which is the high-value application for fly ash, the unburned carbon
needs to be reduced either by optimizing combustion process or by efficient carbon
separation techniques. However, both the disposal and the carbon reduction processes
of fly ash are complicated and required large budget and time in the process.
Therefore, better understanding of high LOI fly ash concrete behavior is crucial to be
capable of using it directly in concrete work without needs of additional process.
This research aims to investigate and clarify the effect of LOI of fly ash on
many basic properties and durability of concrete. To be able to compare the
performances of fly ash concrete containing various %LOI and to vary the %LOI of
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fly ash without any changes in chemical and physical properties, artificial high LOI
fly ashes were made and used throughout this entire study. Low LOI fly ash, having
%LOI of 0.77% from Mae-Moh power plant, Thailand, and powder activated carbon
were used to make other 4 artificial high LOI fly ashes, having %LOI of 6%, 12%,
18% and 25%. Two replacement percentages of fly ash were used at 20% and 40%.
Two different curing conditions, which are air curing and water curing, were used to
investigate the curing sensitivity of high LOI fly ash concrete. Basic properties of low
and high LOI fly ashes such as moisture content, specific gravity, Blaine fineness,
water retainability and water requirement were preliminarily investigated. After that,
experiments on the slump, compressive strength, shrinkage, carbonation and chloride
resistance were carried out. Moreover, slump model and investigation on the
microstructure of low and high LOI fly ash concrete were done for clarifying the test
results.
Moisture content of fly ash increases with the increase of its %LOI. However, the
moisture content of fly ash having %LOI of 25% is still lower than the limit in ASTM
standard specification, which limits the maximum moisture content of fly ash used in
concrete at 3%. Particle size distributions of the prepared high LOI fly ashes are
coarser than the low LOI fly ashes, whereas the Blaine fineness of high LOI fly ashes
are higher. This is because high LOI fly ashes used in this study have more porous
structure and contain irregular particles, because of the added PAC particles. Water
retainability of fly ash increases when %LOI of fly ash increases due to the porous
and rough-texture particles. Therefore, high LOI fly ashes increase the water
requirement of the mixtures.
Using low LOI fly ash significantly improves the slump of concrete compared to
the cement-only mixture. However, slump of fly ash concrete was significantly
affected by the %LOI of fly ash. The initial slump of concrete gradually decreases
with the increase of %LOI of fly ash. Nevertheless, using fly ash having %LOI of
0.77% to 6% with replacement percentage of 20% in the mixture seems to improve
the workability of concrete comparing to the cement-only mixture. Increase percent
replacement of fly ash from 20% to 40% significantly enhances slump of fly ash
concrete having %LOI of 0 to 12%. On the contrary, the slump of concrete with 40%
fly ash replacement gradually decreases and becomes worse than that of 20%
replacement when %LOI of fly ash is over 12%. This phenomenon is because when
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the high amount of high LOI fly ash is used in the mixture, its water retainability
plays the more important role than its lubrication effect.
The reduction in compressive strength of high LOI fly ash concrete was obtained
in the case of the controlled slump by adjustment of water. However, the increase in
compressive strength of high LOI fly ash concrete was obtained in the cases of the
controlled slump by the use of superplasticizer and controlled w/b. In the latter 2
cases, the compressive strength of concrete gradually increases when %LOI of fly ash
increases from 0.77 to 12%. Although the compressive strength tends to gradually
decrease when %LOI of fly ash is beyond 12%, the overall compressive strength of
high LOI fly ash concrete is comparable to fly ash concrete with the lowest %LOI
(LOI=0.77%). Increase the replacement percentage of fly ash from 20% to 40%
resulted in lower compressive strength for mixtures with fly ash with all %LOI. Using
high LOI fly ashes in the mixtures can reduce the curing sensitivity of fly ash
concrete, especially the one that containing %LOI of 12% due to its internal curing
effect. The increase in compressive strength of high LOI fly ash concrete was found
to be due to its internal curing effect. SEM pictures of polished high LOI fly ash
concrete showed that cement paste infiltrated into the rough surface and pores of the
carbon particles. Cement and fly ash react with the additional water, absorbed by the
carbon particles, resulting in better bonding between cement and carbon particles.
Moreover, the result from micro hardness test of high LOI fly ash concrete also
revealed that the hardness values near to carbon particles were higher than those near
to fly ash particles, proofing the existence of hard shell around the carbon particles.
Carbonation and chloride resistances of high LOI fly ash concrete are worse than
the low LOI fly ash concrete. However, the effect of LOI of fly ash was less
significant when using in low w/b concrete. Autogenous shrinkage of high LOI fly
ash was significantly decreased. This result is one of the evidences indicating the
internal curing ability of high LOI fly ash. Total shrinakge of high LOI fly ash
concrete gradually increases with the increase of %LOI of fly ash. However, the use
of fly ash with %LOI of 0.77 to 25% can reduce the total shrinkage when compared to
the OPC mixture.
Keywords: High LOI fly ash, fly ash, water retainability, compressive strength,
curing sensitivity, carbonation, shrinkage
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Table of Contents
Chapter Title Page
Signature Page i
Acknowledgements ii
Abstract iii
Table of Contents vi
List of Figures x
List of Tables xiii
1 Introduction 1
1.1 General 1
1.2 Statement of problems 2
1.3 Objectives 3
1.4 Scope of study 4
2 Literature Review 5
2.1 Fly ash 5
2.1.1 Chemical composition and mineralogical of fly ash 6
2.1.2 Physical properties and morphology of fly ash 7
2.1.3 High LOI fly ash 9
2.2 Standard specifications of fly ash for use in concrete 10
2.2.1 ASTM standard 10
2.2.2 Vietnamese standard 11
2.2.3 Thai standard 13
2.2.4 Japanese standard 13
2.3 Effect of fly ash on concrete properties 14
2.3.1 Effect of fly ash on properties of fresh concrete 14
2.3.2 Effect of fly ash on compressive strength of concrete 16
2.3.3 Effect of fly ash on durability of concrete 19
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3 Experimental Program 22
3.1 General 22
3.2 Materials 22
3.2.1 Cement 22
3.2.2 Fly ashes 22
3.2.3 Activated carbon 24
3.3 PAC selection and preparation 25
3.4 Experimental Methodology 28
3.4.1 Properties of artificial high LOI fly ash 28
3.4.1.1 Loss on ignition 28
3.4.1.2 Water retainability 30
3.4.2 Basic and mechanical properties of high LOI fly ash concrete 31
3.4.2.1 Slump 31
3.4.2.2 Compressive strength 33
3.4.3 Durability 36
3.4.3.1 Autogenous shrinkage 36
3.4.3.2 Total shrinkage 38
3.4.3.3 Carbonation 39
3.4.3.4 Rapid Chloride Penetration Test (RCPT) 41
3.4.4 Microstructure of high LOI fly ash concrete 44
3.4.4.1 Porosity of concrete 44
3.4.4.2 Micro hardness 44
4 Results of Basic Properties of High LOI Fly Ash 47
4.1 General 47
4.2 Morphology of fly ashes and powdered activated carbons 47
(PACs)
4.2.1 Morphology of fly ashes with various %LOI 47
4.2.2 Morphology of powdered activated carbons (PACs) 51
4.3 Properties of artificial high LOI fly ash 53
4.3.1 Basic properties of fly ash 55
4.3.2 Particle size distribution 56
4.3.3 Water retainability 57
4.3.4 Water requirement 58
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5 Results and Clarifications of Slump 59
5.1 Initial slump of concrete 59
5.2 Clarification of slump behavior 61
5.2.1 Background of slump model 61
5.2.1.1 Slope of slump-free water content curve (α) 61
5.2.1.2 Free water content in fresh concrete (Wfr) 62
(1) Water retainability of powder materials (β𝑝) 62
(2) Surface water retainability of aggregates (Wra′ ) 63
(a) Water retainability coefficient of aggregates 63
(βagg′)
(b) Determination of specific surface area of fine 63
and coarse aggregate
5.2.1.3 Minimum free water content required to initiate slump 64
(W0)
(1) Effective surface area of solid particles (Seff) 65
(2) Lubrication coefficient (L) 66
5.2.2 Verification of initial slump of high LOI fly ash concrete 66
6 Results and Clarifications of Compressive Strength 72
6.1 General 72
6.2 Effect of high LOI fly ash on compressive strength of concrete 72
6.2.1 Controlled slump 72
6.2.2 Controlled water to binder ratio 74
6.3 Effect of fly ash content on compressive strength of high LOI 76
fly ash concrete
6.4 Effect of different curing conditions on compressive strength 79
of high LOI fly ash concrete
6.4.1 Controlled water to binder 79
6.4.2 Controlled slump by using superplasticizer 80
6.5 Curing sensitivity of high LOI fly ash concrete on compressive 81
strength
6.6 Microstructure study of high LOI fly ash concrete 83
6.6.1 Porosity of fly ash mortars and concrete with different %LOI 83
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6.6.2 Microstructure examination of high LOI fly ash concrete 85
by SEM
6.6.3 Experiment on micro hardness 88
7 Results of Durability of High LOI Fly Ash Concrete 92
7.1 Effect of high LOI fly ash on carbonation resistance 92
7.2 Effect of high LOI fly ash on chloride resistance 97
7.3 Effect of high LOI fly ash on shrinkage 99
7.3.1 Autogenous shrinkage 99
7.3.2 Total shrinkage 100
8 Conclusions and Recommendations 102
8.1 Conclusions 102
8.2 Recommendations for future studies 105
References 106
Appendices 113
Appendix A 114
Appendix B 116
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List of Figures
Figures Page
2.1 Survey of products containing SiO2, Al2O3 and CaO 6
2.2 Backscattered electron (BSE) images of different fly ash particles 8
2.3 SEM images of unburned carbon particles 10
2.4 Reduction of water demand of fresh concrete with a spread of 42 cm 15
3.1 Fly ash from different sources 23
3.2 Particle shapes of activated carbon (AC) from different sources 24
3.3 Planetary ball mill 26
3.4 Grinding process of powdered activated carbon (PAC) 26
3.5 Schematic outline of this study 27
3.6 Apparatus for LOI test 29
3.7 Mini slump test 30
3.8 Mixture designation nomenclature 31
3.9 Apparatus for slump test 32
3.10 Cube molds having size of 10x10x10 cm for casting concrete 34
3.11 Compressive strength test machine 34
3.12 Bar molds for autogenous and total shrinkage test 36
3.13 Autogenous shrinkage paste specimens 37
3.14 The length comparator used for measuring expansion of 37
the bar specimens
3.15 Bar specimens for total shrinkage test 38
3.16 Specimens after spraying phenolphthalein solution 40
3.17 Cylinder molds 41
3.18 A slice of RCPT specimen 42
3.19 Apparatus for Rapid Chloride Penetration Test 42
3.20 Mold and cube concrete specimens 45
3.21 Concrete cubes inside resin after polishing 45
3.22 Vickers hardness test apparatus 46
4.1 SEM pictures of low LOI fly ash (LOI = 0.77%) 48
from Mae-Moh power station, Thailand
4.2 SEM pictures of high LOI fly ash (LOI = 5.36%) 49
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from BLCP power station, Thailand
4.3 SEM pictures of high LOI fly ash (LOI=18.04%) from Vietnam 50
4.4 EDX result of particle #1, Vietnamese fly ash 51
4.5 SEM pictures of Powdered Activated Carbons (PACs) 52
4.6 Particle size distributions of UC-FV and PAC-BC 53
4.7 SEM pictures of real and artificial high LOI fly ashes 54
4.8 Particle size distributions of cement, fly ashes with various 56
%LOI and PAC produced from bituminous coal
4.9 Water retainability coefficients of fly ashes with various %LOI 57
4.10 Water requirement of mortars containing fly ashes with various %LOI 58
5.1 Initial slump of concrete containing fly ashes with various %LOI 60
(w/b=0.4)
5.2 Initial slump of concrete containing fly ashes with various %LOI 60
(w/b =0.5)
5.3 Predicted slump of low and high LOI fly ash concrete (w/b =0.4) 69
5.4 Predicted slump of low and high LOI fly ash concrete (w/b =0.5) 69
5.5 Water retainability coefficients of fly ashes at with various %LOI 70
5.6 Lubrication coefficient of fly ashes with various %LOI 70
5.7 Relationship between Wfr, W0 and %LOI of fly ash (w/b =0.4) 71
6.1 Compressive strength of OPC and fly ash concrete, containing various 73
%LOI (controlled slump by adjustment of water)
6.2 Compressive strength of OPC and fly ash concrete, containing various 73
%LOI (controlled slump by using superplasticizer)
6.3 Compressive strength of OPC and fly ash concrete, containing various 75
%LOI (20% fly ash replacement, controlled w/b at 0.4)
6.4 Compressive strength of OPC and fly ash concrete, containing various 75
%LOI (20% fly ash replacement, controlled w/b at 0.5)
6.5 Compressive strength of high LOI fly ash concrete with various 77
%replacements of 20 and 40% (w/b =0.4)
6.6 Compressive strength of high LOI fly ash concrete with various 78
%replacements of 20 and 40% (w/b =0.5)
6.7 Compressive strength of high LOI fly ash concrete in 79
different curing conditions (controlled w/b at 0.4)
6.8 Compressive strength of high LOI fly ash concrete in 80
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different curing conditions (controlled slump by using superplasticizer)
6.9 Curing sensitivity of fly ash concrete containing various %LOI 82
for controlled w/b case (w/b=0.4)
6.10 Curing sensitivity of fly ash concrete containing various %LOI 83
for controlled slump at 8.5 cm by using admixture case
6.11 Total volume of permeable voids in fly ash mortars with different %LOI 84
6.12 Total volume of permeable voids in fly ash concrete with different %LOI 84
6.13 ITZ microstructure of high-carbon fly ash lightweight aggregate concrete 86
6.14 Typical view of paste around a particle of fly ash and carbon 87
6.15 ITZ microstructure of a carbon particle and cement paste 87
6.16 Average hardness values near to fly ash particles with their 89
tested locations of concrete containing fly ash with %LOI 0.77%
6.17 Average hardness values near to carbon particles with their 90
tested locations of concrete containing fly ash with %LOI 12%
6.18 Average hardness values near to fly ash particles with their 91
tested locations of concrete containing fly ash with %LOI 12%
7.1 Carbonation depth of fly ash concrete containing various %LOI 93
at different exposure periods, (water-cured condition)
7.2 Carbonation depth of fly ash concrete containing various %LOI 94
at different exposure periods, (water-cured and air-cured condition)
7.3 Curing sensitivity index on carbonation of fly ash concrete 96
containing various %LOI (w/b=0.4), at different exposure periods
7.4 Chloride permissibility of fly ash concrete containing various %LOI 98
by measuring charge passed (w/b=0.4)
7.5 Chloride permissibility of fly ash concrete containing various %LOI 98
by measuring charge passed (w/b=0.5)
7.6 Autogenous shrinkage of pastes containing fly ashes with various %LOI 99
(w/b=0.25)
7.7 Autogenous shrinkage of pastes containing fly ashes with various %LOI 100
(w/b=0.40)
7.8 Total shrinkage of pastes containing fly ashes with various %LOI 101
(w/b=0.25)
7.9 Total shrinkage of pastes containing fly ashes with various %LOI 101
(w/b=0.40)
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List of Tables
Tables Page
1.1 Summary of maximum allowable %LOI of fly ash for use in 3
cement/concrete in different coal-using countries
2.1 Chemical properties requirements for fly ash use as mineral admixtures 11
in Porland cement concrete according to ASTM C618
2.2 Specifications of fly ash for concrete and mortar according to 12
TCVN 10302:2013
2.3 Chemical properties, specification of fly ash according to TIS 2135 13
2.4 Standard specifications of fly ash according to JIS-A 6201-1999 14
3.1 Chemical compositions of cement and fly ash 23
3.2 Physical properties of cement and fly ash 23
3.3 Chemical compositions of powdered activated carbons (PACs) 24
3.4 Mix proportions of concrete for slump test. 32
3.5 Mix proportions of concrete for compressive strength test. 35
3.6 Mix proportions of pastes for autogenous shrinkage and total shrinkage 39
test
3.7 Mix proportions of concrete for carbonation and RCPT test 43
4.1 Actual tested %LOI in the prepared fly ashes 55
4.2 Moisture content, specific gravity and Blaine fineness of fly ashes with 55
various %LOI
5.1 Tested and predicted slump results of fly ash concrete containing 67
various %LOI (w/b =0.4)
5.2 Tested and predicted slump results of fly ash concrete containing 67
various %LOI (w/b =0.5)
6.1 Hardness values near fly ash particles of W40FM0 mixture 89
6.2 Hardness values near carbon particles of W40FM12 mixture 90
6.3 Hardness values near fly ash particles of W40FM12 mixture 91
8.1 Performances of high LOI fly ash compared with low LOI fly ash 102
8.2 Performances of high LOI fly ash mixture compared with 103
cement-only mixture
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Chapter 1
Introduction
1.1 General
At present, fly ash, a by-product from the combustion of pulverized coal in
electricity generating power plant, is increasingly utilized worldwide as a cement
replacement material in concrete industry due to its merits in the sense of improving
many concrete properties, cost reduction of concrete and also reducing environmental
problems. The use of good quality fly ash with optimum amount to partially replacing
cement improves many properties of concrete i.e. increasing workability and
pumpability of fresh concrete, improving long-term compressive strength, reducing
temperature, reducing shrinkage, improving resistance against chloride-induced steel
corrosion, increasing sulfate resistance, reducing risk due to alkali-aggregate reaction,
etc [1-7].
Chemical and physical properties of fly ash vary and depend on type of coal,
fineness of pulverized coal, characteristics of furnace, burning and collecting process,
etc. The variation and inconsistency of its properties are the main issues for utilization
of fly ash in concrete works. To ensure that fly ashes are suitable for use in concrete
works, standard specifications (ASTM [8], TIS [9], JIS [10], TCVN [11], etc) have
been drafted in many countries for their local fly ashes based on chemical
composition, physical properties which includes Loss on Ignition (LOI) percentage.
The %LOI of fly ash represents its approximated amount of unburned carbon content.
The excessive amount of sulfur, freelime and unburned carbon content of fly ash
could adversely affect some of the properties of fly ash concrete [12-14].
Thailand is one of the countries that has been very successful in regard to fly
ash usage in concrete industry. The sources of utilized fly ash in Thailand are from
two major locations, which are Lampang (Mae-Moh) and Rayong (BLCP). Mae-Moh
fly ash has low SiO2 content, but high in CaO which contributes to the high
compressive strength of Mae-Moh fly ash concrete. Moreover, not only low in LOI
amount, majority of its particles are in spherical shape, which helps to decrease water
demand of mixtures and therefore enhance workability of fresh concrete [15]. The
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low LOI of Thai fly ash is considered to be due to high allowable burning temperature
of the coal powder in Thailand [16].
1.2 Statement of problems
The proportion of low LOI fly ash is decreasing worldwide as an indirect result
of controlling toxic gases such as nitrogen oxides (NOx) to meet the emission
standards of the 1990 Clean Air Act amendments [17]. More recent coal power plants
around the world, including BLCP power plant, Thailand, are equipped with low-
NOx burners in their boilers, which are operated at lower firing temperature. This
example of approach has an adverse effect on the quality of the produced fly ash due
to the increasing amount of residual unburned carbon in the fly ash. Additionally,
activated carbon, injected to control mercury emission from coal-fired combustion
systems, can increase the carbon level in fly ash even more [18]. The maximum Loss
on Ignition (LOI) for different coal-using countries shown in Table 1.1 demonstrates
that apart from China and Russia, which allow for relatively high LOI values for
certain ashes, the other major coal-consuming countries stipulate similar lower LOI
limits for fly ash use in concrete production due to the fact that high LOI fly ash is
generally known to cause some malfunctions in concrete, which are probably known
to include discoloration, poor air entrainment ability, more water requirement and low
compressive strength [13],[14],[19].
High level of unburned carbon in fly ash hinders its further utilization in
cement and concrete industry. In 2006, 40 million tons of high LOI fly ash in the
United States was placed in landfills [18]. Disposal of fly ash is not only wasteful
manner of potential valuable resources but also money for transportation and disposal
charges. Moreover, it leads to environmental problems [20]. Some amount of high
LOI fly ash and other off-spec fly ash are utilized in low-value method such as using
as a landfill material, soil improvement, road base and raw material for producing
cement. The most effective use of fly ash at present, considering both volume and
value, is still in the area of concrete. So, in order to utilize these high LOI fly ashes in
the concrete work, the unburned carbon, which is an undesirable component, needs to
be reduced either by optimized combustion process or by efficient separation
techniques [21-25].
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Both the disposal and the carbon reduction processes of fly ash are difficult
and required large budget and time in the process. Therefore, better understanding of
high LOI fly ash concrete behavior is crucial to be capable of using it directly in
concrete work. However, it is also clear that the absolute quantity of unburned carbon
alone is not sufficient to judge the suitability of a fly ash for use in concrete
production. To determine precisely that suitability, the actual morphological
properties of high LOI fly ash need to be taken into account. Some studies found that
high carbon content did not have any detrimental influence on the concrete mixture.
Since fly ash having higher %LOI is finer than that having lower LOI. So it might be
the fineness that contributes high strength to the mix and cover the effect of carbon in
fly ash [26-27]. Moreover, a study by Coppola [28] indicated that fly ash with the
highest LOI content (11.30%) performed significantly better than the fly ash with the
lowest LOI content (4.19%) in term of concrete compressive strength development.
Table 1.1 Summary of maximum allowable %LOI of fly ash for use in
cement/concrete in different coal-using countries [20]
Countries LOI limits, %, maximum
Australia 3-6
Canada 3-10
China 5-15
EU
Type A: 5
Type B: 2-7
Type C: 4-9
India 5
Thailand 6
Japan 3-8
Russia Basic ash: 3-5
Acid ash: 2-25
South Africa 5
USA Class F: 6 (12)
Class C: 6
1.3 Objectives
According to the above discussion, the aims of this project are as follows:
To investigate the effects of LOI of fly ash on mechanical properties and
durability of concrete.
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To clarify and be able to explain the behavior of high LOI fly ash, when
its %LOI increase from low to high.
1.4 Scope of study
For the scope of this study, various parameters are studied within the following
scopes.
a) Materials
Type of cement: Ordinary Portland Cement Type I
Type of fly ash: - an original low LOI fly ash (high CaO) from Mae-Moh
power plant, having %LOI of 0.77%
- 4 artificial high LOI fly ashes synthesized by the
blending of low LOI fly ash and powdered activated
carbon (PAC), having different %LOI of
approximately 6%, 12%, 18% and 25%.
b) Paste mixtures
Water to binder ratio: 0.25 and 0.40
Amount of fly ash: 20%
c) Concrete mixtures
Water to binder ratio: 0.4 and 0.5
Amount of fly ash: 0%, 20% and 40% by weight of total binder
d) Experimental programs
Water requirement of mortar
Slump
Compressive strength
Autogenous shrinkage
Total shrinkage
Carbonation
Rapid chloride penetration test
Porosity of concrete
Micro hardness
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Chapter 2
Literature Review
2.1 Fly ash
Fly ash, the most commonly used pozzolan in concrete, is a by-product from
the combustion of pulverized coal in electricity power plants. In addition to
economics and ecological benefits, the use of fly ash in concrete is generally known
to improve many properties of fresh and hardened concrete.
Pozzolans are siliceous or siliceous and aluminous materials which them
selves process little or no hydration reaction. However, in a finely divided form, these
substances can chemically react with the calcium hydroxide in the presence of
moisture to form the compounds that have cementitious properties (ASTM standard
C618-80). This reaction is called the pozzolanic reaction. Fly ashes act as pozzolanic
materials when mixed with portland cement and water, by reacting with the calcium
hydroxide released by the hydration of Portland cement to produce various calcium-
silicate hydrates (C-S-H) and calcium-aluminate hydrates. Some fly ashes with higher
amounts of calcium will also display cementitious behavior by reacting with water to
produce hydrates in the absence of a source of calcium hydroxide. These pozzolanic
reactions are beneficial to the concrete in that they increase the quantity of the product
of cementitious binder phase (C-S-H) and, to a lesser extent, calcium-aluminate
hydrates, improving the long term strength and reducing the permeability of the
system. Both of these mechanisms enhance the durability of the concrete [29].
Since fly ash is a by-product, its properties depend on many factors such as:
the characteristics of its origin coal, combustion system design and operating
conditions, collecting process, etc. The performance of fly ash in concrete is greatly
influenced by its physical, mineralogical and chemical properties. Fly ashes can be
used in the concrete industry if its properties conform to the standard specifications
for fly ash used in concrete.
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2.1.1 Chemical composition and mineralogical of fly ash
The chemical composition and mineralogical properties of fly ash depend
mainly upon the composition of original coal and combustion method. Generally, the
chemical composition of fly ash shows a wide diversity, but the major chemicals of
fly ash are SiO2 (25-60%), Al2O3 (10-30%), Fe2O3 (5-25%), CaO (1-35%). Figure 2.1
shows the position of fly ash with low calcium content in the ternary diagram SiO2-
Al2O3-CaO. Fly ashes can be classified into two groups as class C and class F
according to ASTM C-618. Class C fly ash, originated from lignitic coal, vastly has
CaO content higher than 10% and the sum of SiO2, Al2O3, Fe2O3 is higher than 50%.
Class F fly ash is originated from anthracite or bituminous coal. It consists of less
than 10% CaO and the sum of the major oxides is higher than 70%. The fly ash
generated recently tends to have lower value of SiO2 and higher carbon content [30].
Figure 2.1 Survey of products containing SiO2, Al2O3 and CaO [31]
Fly ash is a complex material consisting of heterogeneous combinations of
amorphous (glassy) and crystalline phases. The largest fraction of fly ash consists of
glassy spheres of two types, solid and hollow (cenospheres). These glassy phases are
typically 60 to 90% of the total mass of fly ash. The remaining fractions of fly ash are
made up of a variety of crystalline phases. These two phases are not completely
separated and independent of one another [32]. Unburned carbon particles are
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collected with the fly ash as particles of carbon, which may constitute up to 16% of
the total. The amount of unburned carbon in fly ash depends on the rate and
temperature of combustion, the degree of pulverization of the original coal, the
fuel/air ratio, the nature of the coal being burned, etc [33].
The carbon content in fly ash is a result of incomplete combustion of the coal
and organic additives used in the collection process. Carbon content is not usually
determined directly, a generally accepted test method for estimating the unburned
carbon content of fly ash is the determination of its loss on ignition or LOI [34].
However, in the LOI test method, it has been observed that LOI result may
overestimate the amount of the unburned carbon [35-36] as the ignition mass loss is
not only due to burning of organic carbon but also due to other possible reactions such
as calcination of inorganic carbonates, desorption of physically and chemically bound
water (e.g., dehydration of portlandite), and oxidation of sulfur and iron mineral. In
contrary, the presence of sulphides, sulphur, and some iron minerals will decrease the
LOI value due to gain in weight because of oxidation. However, the carbon seems to
be the substance most responsible for ignition loss [37]. Fly ash used in concrete
typically has %LOI less than 6%; however, ASTM C 618 mentions that the use of
class F fly ash with %LOI up to 12% can be used, if either acceptable performance
records or laboratory test results are made available.
2.1.2 Physical properties and morphology of fly ash
The morphology of fly ash particles is controlled by both the combustion
temperature and cooling rate. Fly ash can exist as round particles, angular particles,
cenospheres, plerospheres, broken pieces of coarser particles, or fused particles.
Generally fly ash comprises of spherical solids and hollow cenospheres [38]. The
majority of fly ash particles ranged in size from approximately 1 to 100 μm and
consisted of small solid spheres (Figure 2.2A), hollow cenospheres (Figure 2.2B),
irregularly shaped unburned carbon particles (Figure 2.2C), minerals and mineral
aggregates, such as the quartz (Figure 2.2D), agglomerated particles (Figure 2.2E) and
irregularly shape amorphous particles (Figure 2.2F). These physical properties of fly
ash such as particle shape, fineness, particle-size distribution, and density of fly ash
particles influence the properties and performances of fresh and hardened concrete.
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Lane and Best [40] reported that the shape of fly ash particles is also a function
of particle size. The majority of fly ash particles are glassy, solid, or hollow, and
spherical in shape. Examples of fly ash particle shapes are shown in Figures 2.2 and
2.3. Fly ash particles that are hollow are translucent to opaque, slightly to highly
porous, and vary in shape from rounded to elongated.
Figure 2.2 Backscattered electron (BSE) images of different fly ash particles
(A) typical fly ash spheres; (B) hollow cenosphere in cross-section; (C) unburned
carbon particle; (D) mineral aggregate (quartz); (E) agglomerated particles in cross-
section; (F) irregularly shaped amorphous particles [39].
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Styszko-Grochowiak et al [41] studied about characterization of the coal fly ash
for the purpose of improvement of industrial on-line measurement of unburned carbon
content. The conclusion of the study was found that the content of unburned carbon is
closely linked to the particle size distribution of fly ash. The content of unburned
carbon diminishes with the smaller size of particles of the fly ash.
2.1.3 High LOI fly ash
High LOI fly ash means fly ash that contains high amount of unburned carbon
content, since carbon is generally the substance most responsible for ignition loss
[37]. The terms loss on ignition (LOI) and content of carbon are often used
interchangeably. A generally acceptable test method to initially estimate the unburned
carbon content of fly ash is the determination test of its loss on ignition, or LOI test
(ASTM D7348). However, this test is not sufficient to identify the suitability of a fly
ash for the concrete industry, since this test only give an approximation to the carbon
content of a sample and provides no information about the form or properties of
carbon [13].
The factors affecting unburned carbon content or %LOI of fly ash were found to
come from these 2 major groups, which are the effect of coal characteristics and the
effect of combustion system design and operating conditions [42]. Moreover, the
widespread installation of low-NOx combustion systems is one of the most significant
problems in terms of increasing %LOI of fly ash. Higher level of %LOI of fly ash
hinders its further utilization in concrete industry, due to its drawbacks in fresh and
hardened concrete properties.
The unburned carbon particle (Figure 2.3a) has a porous structure. Some
spherical particles are attached to the external surface, and some are penetrated inside
the cavities and large pores of the unburned carbon particles (Figure 2.3b). The
variety in particle shape and pore structure of unburned carbon particles of fly ash
might be achieved depending on the 2 main factors mentioned above. The porous
characteristic of unburned carbon particles provides them a very good absorptive
ability. Freeman [13] found that hydrophobic end of air entraining agent (AEA),
which is used to stabilize air bubbles in concrete, is attached on carbon surface area
consisting of the external surface of carbonaceous particle and some internal surfaces
of larger pores. This results in rendering them unavailable for attachment to air
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bubbles and this low-entrained-air concrete will have less resistance to freezing and
thawing cycles. Other effects of those unburned carbon content of fly ash on
properties of concrete are known to include discoloration, poor air entrainment ability,
high water requirement, low compressive strength and mixture segregation.
(a) x250 (b) x3000
Figure 2.3 SEM images of unburned carbon particles [43]
2.2 Standard specifications of fly ash for use in concrete
2.2.1 ASTM standard
There are various schemes of fly ash classification. In the United States, the
specification which is used for evaluating suitability of fly ash is ASTM C618 [8],
“Standard Specification for Coal Fly Ash and Raw or Calcined Natural Pozzolan for
Use in Concrete”. This specification classifies fly ash into two major classes i.e. class
C and class F based on the chemical composition and the initial coal (Table 2.1).
Generally, class F is the result of combusting anthracite or bituminous coal while
class C fly ash is formed by combustion of lignite or sub-bituminous coal. LOI
represents the amount of unburned carbon in fly ash. As existing carbon is not ideal
for concrete especially in terms of air entraining, LOI is limited to 6% by ASTM.
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Table 2.1 Chemical properties requirements for fly ash used as mineral admixtures
in Portland cement concrete according to ASTM C618
Characteristic Requirements
Class F Class C
SiO2+Al2O3+Fe2O3, min % 70 50
SO3, max % 5.0 5.0
Moisture content, max % 3.0 3.0
LOI, max % 6.0 6.0
2.2.2 Vietnamese standard
According to TCVN 10302, which is the specification of fly ash for concrete
and mortar in Vietnam, fly ashes are also classified into 2 major classes, which are
class F and class C fly ashes (Table 2.2). The classification of Vietnamese fly ash
specification is based on the chemical compositions of fly ash such as: the total
summation of the 3 major chemical constituents of fly ash, sulfur, free calcium oxide
and LOI percentage of fly ash. Moreover, specification of fly ash in Vietnam also
classified fly ash into 5 groups, by considering the applications level of the fly ash.
- Application a: for reinforced concrete products and components made
from normal concrete and lightweight concrete
- Application b: for non-reinforced concrete products and components made
from normal concrete, lightweight concrete and mortar
- Application c: for concrete products and components made from cellular
concrete
- Application d: for reinforced concrete products and components exposed
to special conditions.
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Table 2.2 Specifications of fly ash for concrete and mortar according to TCVN
10302:2013 [11]
Characteristics Fly ash
type
Application level
a b c d
1. Total oxides (SiO2+Al2O3+Fe2O3), %
mass, Min.
F
C
70
45
2. Sulfur trioxide SO3, % mass, Max. F
C
3
5
3
5
3
6
3
3
3. Free calcium oxide CaO, % mass, Max. F
C
-
2
-
4
-
4
-
2
4. Loss on Ignition (LOI), % mass, Max. F
C
12
5
15
9
8*
7
5*
5
5. Harmful alkali (soluble alkali), % mass,
Max
F
C 1.5
6. Moisture content, % mass, Max. F
C 3
7. Retaining on 45m sieve, % mass, Max. F
C 25 34 40 18
8. Water demand over control, % mass, Max. F
C 105 105 100 105
9. Content of ion Cl-,% mass, Max F
C 0.1 - - 0.1
10. Natural radioactivity Aeff, (Bq/kg) of fly
ash for:
- Civil, public building, Max.
- Industrial building, urban and municipal
road, Max
370
740
* When burning anthracite coal, fly ash with LOI up to 12% and 10% maybe approved
for the applications c and d, respectively according to the agreement with users or
accepted laboratory testing results.
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2.2.3 Thai standard
According to TIS 2135 [9], “Coal fly ash for use as an admixture in concrete”,
Thai Industrial Standards Institute, fly ashes used in concrete are classified into 3
classes: class 1, class 2 and class 3 (Table 2.3). Most of the fly ashes are in class 2
which are separated into types 2a and 2b. Class 2a requires percentage of calcium
oxide (CaO) less than 10 %, whereas class 2b contains CaO not less than 10 %.
Table 2.3 Chemical properties, specification of fly ash according to TIS 2135 [9]
Item Properties
Requirement
Class 1 Class 2 Class 3
Type a Type b
1 Silicon dioxide (SiO2), min % 30.0 30.0 30.0 30.0
2 Calcium oxide (CaO), % - Less than
10.0
Not less
than 10.0
-
3 Sulfur trioxide (SO3), max% 5.0 5.0 5.0 5.0
4 Moisture content, max % 3.0 3.0 2.0 12.0
5 LOI content, max % 6.01) 6.01) 6.01) 6.01)
2.2.4 Japanese standard
The Japan Industrial Standard (JIS) A 6201 [10], “Fly Ash for Use in
Concrete,” classifies fly ash as Types I, II, III, and IV (see Table 2.4) mainly on their
%LOI and fineness described as follows:
• High-quality fly ash with LOI less than 3.0% and Blaine fineness higher than
5000 cm2/g is specified as Type I.
• Most of the fly ash qualified in JIS A 6201-1996 is specified as Type II.
• Fly ash with high LOI ranging from 5.0 to 8.0% is specified as Type III.
• Fly ash with low Blaine fineness ranging from 1500 to 2500 cm2/g is specified
as Type IV.
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Table 2.4 Standard specifications of fly ash according to JIS-A 6201-1999
Item Type I Type II Type
III Type IV
Silica dioxide (%) 45.0 or higher
Moisture content (%) 1.0 or less
Ignition Loss (%) 3.0 or
less
5.0 or
less
8.0 or
less
5.0 or
less
Density (g/cm3) 1.95 or higher
Fineness
Residue on 45m sieve
(screen sieve method) (%)
10 or
less
40 or
less
40 or
less
70 or
less
Specific surface area (Blaine
method) (cm2/g)
5000 or
higher
2500 or
higher
2500 or
higher
1500 or
higher
Flow value ratio (%) 105 or
higher
80 or
higher
80 or
higher
60 or
higher
Activity
index
(%)
Material age: 28 days 90 or
higher
80 or
higher
80 or
higher
60 or
higher
Material age: 91 days 100 or
higher
90 or
higher
90 or
higher
70 or
higher
2.3 Effect of fly ash on concrete properties
2.3.1 Effect of fly ash on properties of fresh concrete
Owens [44] reported that the use of fly ash containing a larger fraction of
particles coarser than 45μm or a fly ash with high amount of unburned carbon and
loss on ignition more than 1% resulted in higher water demand.
Lewandowski [45] reported that the reduction of the water demand of concrete
with a constant spread of 42 cm was distinctly greater for fly ash with an ignition loss
of 3.6 % by mass than for an ignition loss of 9.3% by mass (Figure 2.4)
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Figure 2.4 Reduction of water demand of fresh concrete with a spread of 42 cm due
to substitution of fly ash for Portland cement Z 35 fly ashes with loss on ignition of
3.6% (F3) and 9.3% (F9) [45]
Siddique [46] investigated the effect of fly ash on slump of fresh concrete.
Most of the tested fly ashes were class F type with %LOI of 1.9%, replacing Portland
cement with three percentages (40%, 45%, and 50%). When fly ash content of
mixtures increased, their slump increased. On the other hand, slump of fresh concrete
with fly ash was higher than that of cement only.
Amonamarittakul [15] conducted a research using one fly ash from Mae-Moh
power plant and 4 fly ashes from BLCP power plants. Mae-Moh fly ash is high CaO
fly ash with very low %LOI of 0.14% while BLCP fly ashes are low CaO fly ashes
having %LOI from 2.57%, 3.29%, 3.78% and 4.09%. It was found that low LOI
content and spherical particles shape of fly ash can reduce water requirements of fly
ash concrete. Fly ash that has the lowest LOI content and most spherical particle
shape requires less water than other fly ashes to obtain the same water requirement of
mortar and slump of concrete.
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2.3.2 Effect of fly ash on compressive strength of concrete
Hornain [26] investigated the effect of residual carbon content in fly ash on the
hardened cement paste properties. Fly ashes with three percentages residual carbon
were used: 4, 7, and 12%. The order of fineness is the fly ash with 12, 7, and 5%.
Their results show that strength of fly ash with 12% is not different from that with 7
and 5% and is lower than that of the normal cement specimens. The strength of these
fly ash mortars increase with time. They conclude that the high carbon content did not
have any detrimental influence on strength of the concrete mixture. Since fly ash with
12% is finer than 5% so it might be this fineness that contributes high strength to the
mix and covers the effect of carbon in the fly ash. In order to investigate the effect of
carbon on strength, the fly ashes used for testing should have the same fineness.
Bumrongjaroen, W [30] studied about utilization of processed fly ash in mortar.
Several types of fly ashes, which are wet bottom, dry bottom and low NOx fly ashes
were used. The fly ash from the original feed of dry bottom ash and wet bottom ash
have LOI about 2.05 to 4.57% of carbon, while the fly ash from low NOx ash has LOI
of about 12.5% of carbon. All fly ashes were ground to different particle size
distributions. It was found that the grinding method is an effective means to process
raw wet bottom, dry bottom, and low NOx fly ash in to beneficial products. The
quality of fly ash increases significantly after grinding. With cement replacement up
to 42%, the strength of ground fly ash mortar performed as well as or better than plain
cement mortar after 14 days. It was proved that ground fly ash increases the strength
properties of mortar because its fineness enhances the three mechanisms operating for
strength gain: dispersion, nucleation, and pozzolanic activity. The dispersion function
of fly ash was observed from the pore size distribution of the 5-minute paste. When
fly ash was present, the cement grains were more dispersed, resulting in a finer pore
size distribution. The pore size reduction at age of 28 days could be a result of both
nucleation and pozzolanic action. The evidence of nucleation is the thicker hydration
products on fly ash particles and the evidence of pozzolanic action are the
deterioration in some fly ash particles as well as the depletion of calcium hydroxide
content. It was also found that the ground fly ash mortar with high carbon content
performs better than that of normal mortar and the ground fly ash mortar without
carbon.
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Fox and Constantiner [47] studied the influence of fly ash after change to Low-
NOx Burners (LNB) on concrete strength. Samples of fly ash before and after the
change to LNB were collected at a plant consistently burning southern lignite from
one mine. The strength activity index according to ASTM C311, affinity for air-
entraining admixtures, chemical composition, particle size and shape, glass content,
and phase assemblage by quantitative x-ray diffraction were tested. Strength activity
index at 3, 7, 28 and 56 days for low-NOx fly ash were consistently 10% lower than
the corresponding values for the fly ash before the burner change. There is no
significant change in chemical composition between samples taken before and after
the LNB installation. Fly ash produced after LNB went online has slightly higher
active carbon contents, more coarse particles, and slightly less glass, which can
explain the reduction of its strength activity index.
Amonamarittakul [15] conducted a research using one fly ash from Mae-Moh
power plant and 4 fly ashes from BLCP power plants. Mae-Moh fly ash is high CaO
fly ash having CaO content of 20.91% and very low %LOI of 0.14% while BLCP fly
ashes are low CaO fly ashes having CaO in range between 0.75% to 2.13% and %LOI
from 2.57%, 3.29%, 3.78% and 4.09%. The results found that regarding chemical
composition, CaO content is an important parameter that has influence on the early
age strength development. The early age compressive strength of high CaO fly ash
(Mae-Moh fly ash) is higher than that of the low CaO fly ash. However, compressive
strength of low CaO fly ashes from BLCP power plant are slightly higher than that of
the Mae-Moh fly ash at later ages due to the higher dissolution content of pozzolanic
materials (SiO2, Al2O3).
Siddique [48] studied the strength of concrete containing class F fly ash with
%LOI of 1.9%, using 3 replacement percentages, which are 40%, 45%, and 50%. It
was found that all replacement percentages of fly ash reduced the compressive
strength of concrete at 28 days, but there was a continuous and significant
improvement of strength properties beyond 28 days. However, the strength of
concrete with 40%, 45% and 50% fly ash content at 28 days is sufficient for use in
reinforced cement concrete construction.
Cengiz Duran Atis [19] studied the effect of LOI in high volume fly ash
concrete made with and without superplasticizer. The experiment was conducted
using two fly ashes from the electricity generating Drax and Aberthaw power stations
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in England. The %LOI of Drax and Abethaw fly ashes are of 2.80% and 15.60%,
respectively. Fly ashes were used to replace cement with replacement levels of 50 and
70 mass %. The results of this study showed that Drax fly ash had the ability to
reduce the water demand of a concrete mixture. Aberthaw fly ash, which is a high
LOI fly ash, increased the water demand of concrete due to its high LOI content. In
term of compressive strength, Drax fly ash developed higher strength than the
Aberthaw fly ash. The concrete containing 50% Drax fly ash developed high strength,
while 70% fly ash replacement concrete developed moderate strength. Using fly ash
replacement of 50%, Aberthaw fly ash developed satisfactory strength at 28 days and
high strength at 1 year.
Coppola et al [28] studied compressive strength of concrete using four fly ashes
(A, B, C, D). Fly ash A and D came from two different coal fired generating plants,
whereas fly ash B and C were produced by mixing the other two materials. The main
difference between these products is the LOI level, which change from a minimum
level of 4.19% for the fly ash A up to a maximum of 11.3% for fly ash D. The
increase in the LOI level was accompanied by a decrease in the specific gravity which
changed from 0.68 kg/l for the fly ash D to 0.88 kg/l for the fly ash A. Two reference
mixtures, without fly ash, were produced with the same amount of mixing water
(200kg/m3) and different cement factors, 417 kg/m3 and 294 kg/m3, for the reference
concrete R1 and R2, respectively. Therefore, the adopted w/c was 0.48 and 0.68 for
the reference mixtures R1 and R2, respectively. A naphthalene base superplasticizer
was used in concrete containing fly ash B, C and D in order to obtain approximately
the same slump level (180-200mm) as the reference mixtures. It was surprising to
record that there was no relationship between the fly ash LOI content and the concrete
compressive strength development. As a matter of fact, the fly ash D with the highest
LOI content (11.30%) performed significantly better than the fly ash A with the
lowest LOI content. This could be ascribed to the specific composition of fly ash D,
which acted as a better pozzolan in spite of higher amount of the LOI material.
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2.3.3 Effect of fly ash on durability of concrete
Sudsangium [49] investigated the applicability of Mae-Moh fly ashes which
contain different SO3 contents as a solution to reduce autogenous shrinkage and
compared them with a fly ash from Hong Kong. The effect of autogenous shrinkage
in terms of compressive strength, flexural strength and setting of cement pastes with
and without Mae-Moh fly ashes and fly ash from Hong Kong were examined. From
the test results, it was concluded that under sealed condition, fly ashes could be used
for reducing autogenous shrinkage by their spherical particles which led to larger free
water content and SO3 content of Mae- Moh fly ashes. The higher SO
3 content is, the
larger autogenous shrinkage reduction was obtained. Mae- Moh fly ashes were more
effective in improving compressive strength and flexural strength than the fly ash
from Hong Kong.
Tangtermsirikul [50] studied the effect of fly ashes with various chemical
compositions, particle sizes and replacement percentages on autogenous shrinkage of
the pastes with fly ashes. It was found that for the effect of chemical composition, fly
ash with higher SO3 content resulted in lower autogenous shrinkage. For the effect of
particle size, paste with fly ash having smaller average size than cement exhibited
larger autogenous shrinkage whereas pastes with fly ash having bigger size than
cement showed smaller autogenous shrinkage than that of the reference cement paste.
For the effect of fly ash content, non- classified and classified fly ash having larger
average size than cement showed the same tendency i.e. larger autogenous shrinkage
in 20% fly ash paste than in 50% fly ash paste when non-classified fly ash was used.
On the other hand, smaller autogenous shrinkage in 20% fly ash paste than in 50% fly
ash paste was found in case of pastes with classified fly ash having smaller average
size than cement. It could be concluded that not only chemical composition which
affects rate of hardening and volume change of pastes with fly ash but also particle
size, which affects the pore structure of the paste, has to be considered for modeling
autogenous shrinkage of pastes with fly ash.
Tongaroonsri [51] indicated that spherical shape of fly ash particles seemed to
be the main factor that caused less water retainability than the irregular cement
particles did. This resulted in larger free water content in the mixtures with fly ash
than in the mixtures without fly ash when prepared with the same w/b. As autogenous
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shrinkage is the result of water consumption in the hydration process, larger free
water content can reduce the shrinkage. Moreover, pozzolanic reaction of fly ash
proceeds slowly. Also when a part of cement is replaced by fly ash, the cement
hydration reaction is retarded.
Subsomboon [52] studied the effect of Mae-Moh fly ash on shrinkage and
swelling of cement paste. The specimens were controlled, by using replacement
percentages of fly ash at 0, 30 and 50%. The results revealed that the drying shrinkage
decreased by increasing replacement percentage of fly ash.
Pacheerat [53] studied the effect of water to binder ratio and replacement
percentage of fly ash on the length change including the comparison of length change
between mortar and concrete. Fly ash was used at 0, 15, 30, 45 and 60% replacement
by weight of cement run on a series of water to binder ratios at 0.35, 0.50 and 0.65.
From the test results, it was found that the length change of concrete showed the same
trend as mortar but the values were lower for all mixes. When increasing water to
binder ratio, the expansion and drying shrinkage increased while autogenous
shrinkage decreased. When increasing replacement percentage of fly ash, all length
changes decreased.
Chindaprasirt et al. [54] studied the influence of fly ash on water demand and
some properties of hardened mortars. In addition to the original fly ash (OFA), five
different fineness values of fly ash were obtained by sieving and by using an air
separator. The fly ash dosage of 40% by weight of binder was used for the entire
experiment. It was found that the compressive strength of mortar containing fine fly
ash was better than that of original fly ash mortar at all ages. The mixture containing
very fine fly ash gives the highest strength. Although, the use of all fly ashes with all
fineness was significantly reduced the drying shrinkage, the mixture containing coarse
fly ash showed the least improvement. The results of the study suggested that using
fine fly ash resulted in a denser cement matrix and better mechanical properties of
mortar, since it is more reactive.
Ho and Lewis [55] found that the influence of using fly ash as a replacement
material in concrete increased the rate of carbonation due to increasing of porosity in
concrete.
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Khunthongkeaw et al [56] studied carbonation of concrete by using two types of
fly ash with different CaO contents. The decreased ratio of water to binder and fly ash
content led to a better carbonation resistance. For the same fly ash content, specimens
with high-CaO fly ash showed a better carbonation resistance than those of low-CaO
fly ash. This is partly because the tested mixtures with high-CaO fly ash (FA2)
exhibited a lower porosity. Also pH was higher than those with low-CaO fly ash
(FA1) [57]. The results also revealed that when the samples incorporated 10% of fly
ash in the binder, the carbonation coefficients only slightly increased from the
cement-only sample. This increment was drastic when the fly ash content was higher
than 30%. At the fly ash content of 50%, the carbonation coefficient was
approximately two to three times as large as that of the cement-only mixture.
T.-H Ha et al [14] studied the effect of unburned carbon on the corrosion performance
of fly ash mortars. The study used carbon admixed fly ash in order to vary the
percentage LOI of fly ash from 2 to 24%. The results found that the increase in
activated carbon content accelerated the corrosion of rebars in ordinary Portland
cement (OPC) mortars containing fly ash with different percentages of carbon. The
alkalinity of the cement was greatly affected with increased carbon content, and when
the quantity of carbon was increased, cement lost its characteristic color. More than
60% area of rebar steel was rusted. The study suggested that the upper limit of
replacement for various admixed carbon system, under aggressive alternate wetting
and drying condition with 3% NaCl, was 6-8%.
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Chapter 3
Experimental Program
3.1 General
In order to investigate the effect of high LOI fly ash on properties of concrete,
artificial high LOI fly ashes with LOI levels of 0, 6, 12, 18 and 25%, prepared by
blending low LOI fly ash with powdered activated carbon (PAC), were used as a
cement replacing material throughout the entire experiment. The ratio of paste volume
to void volume of aggregate phase of 1.4 was used for all mixtures. In this study, fine
aggregate was natural river sand and coarse aggregate was crushed limestone with a
maximum size of 20 mm. The properties of aggregate complied with the requirement
of ASTM C33 [58]. The specific gravities of fine and coarse aggregates based on
saturated surface dry condition (SSD) were 2.59 and 2.83, respectively (Appendix A).
The ratio by volume of sand to total aggregate of 0.43 giving a minimum void ratio of
0.23 was selected for mix proportions of concrete.
3.2 Materials
3.2.1 Cement
Ordinary Portland cement type I was used. Chemical composition and physical
properties of the cement are shown in Tables 3.1 and Table 3.2, respectively.
3.2.2 Fly ashes
Low LOI fly ash from Mae-Moh power plant was used as a cement replacing
material. Mae-Moh fly ash could be classified as class F fly ash according to ASTM
C618 and class 2b according to TIS 2135. Chemical composition and physical
properties of a Mae-Moh fly ash sample are shown in Tables 3.1 and 3.2,
respectively. Figure 3.1a shows a picture of Mae-Moh fly ash.
In order to make artificial high LOI fly ashes, it is important to know how the
unburned carbon particles in the real high LOI fly ash actually are. Thus, the
characteristic of 2 high LOI fly ashes, one from BLCP power plant, Thailand (see
Figure 3.1b) and another one from a Vietnamese power plant (Figure 3.1c) were
investigated. The high LOI fly ash from Vietnam was used in this experiment as the
archetype for making artificial high LOI fly ashes.
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(a) Mae-Moh (b) BLCP (c) Vietnam
Figure 3.1 Fly ash from different sources
Table 3.1 Chemical compositions of cement and fly ash
Chemical composition Cement Mae-Moh fly ash
SiO2 18.93 35.71
Al2O3 5.51 20.44
Fe2O3 3.31 15.54
CaO 65.53 16.52
MgO 1.24 2.00
Na2O 0.15 1.15
K2O 0.31 2.41
SO3 2.88 4.26
LOI 1.89 0.77
Freelime - 1.71
Table 3.2 Physical properties of cement and fly ash
Physical properties Cement Mae-Moh Fly ash
Specific gravity 3.15 2.21
Blaine fineness (cm2/g) 3100 2867
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3.2.3 Activated carbon (AC)
Powdered Activated Carbons (PACs) used in this experiment were selected
from 3 different available sources of activated carbon in Thailand (Figures 3.2a to
3.2c) i.e coconut shell (CS), bituminous coal (BC) and wood (W). The shape of
activated carbon produced from coconut shell and bituminous coal are granular while
the activated carbon produced from wood is powdery. Therefore, the granular
activated carbon were ground to powder. The LOI of PACs from coconut shell,
bituminous coal and wood were 85.28%, 86.18%, and 80.37%, respectively.
Chemical compositions of all PACs tested by X-ray fluorescence (XRF) are shown in
Table 3.3. PAC selection was considered based on their physical properties,
especially the particle shape characteristic by Scanning Electron Microscopy (SEM).
Table 3.3 Chemical compositions of powdered activated carbons (PACs)
Chemical composition PAC-CS PAC-C PAC-W
SiO2 0.39 3.82 1.10
Al2O3 0.14 1.54 0.31
Fe2O3 0.10 0.36 2.89
CaO 0.16 0.25 0.36
MgO 0.21 - 0.59
Na2O 0.55 - 0.19
K2O 1.61 - 1.05
SO3 - 0.90 0.31
LOI 85.28 86.18 80.37
(a) AC-CS (b) AC-BC (c) AC-W
Figure 3.2 Particle shapes of activated carbon (AC) from different sources
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3.3 PAC selection and preparation
In PAC selection process, carbon content of each fly ash and PAC was
determined by the loss on ignition (LOI) test. Particle shape and pore structure of all
fly ashes and PACs, were investigated by Scanning Electron Microscopy (SEM).
Only the PAC that is the most similar, mainly in term of particle shape and pore
structure, to the unburned carbon particles of Vietnamese fly ash (UC-FV) was
selected.
After the suitable PAC was selected for making artificial high LOI fly ashes, it
was ground to have similar particle size distribution to the unburned carbon particles
of Vietnamese fly ash by using the planetary ball mill (see Figure 3.3). The grinding
procedure of powdered activated carbon was accordingly processed as shown by the
flowchart in Figure 3.4. The grinding parameters consist of rotational speed (rpm),
grinding time, grinding repetitions and quantity of mill balls. In this study, 100g of
PAC were ground each time with 25 mill balls at a rotational speed of 500 rpm for 5
minutes. The grinding repetition was done for 3 times. Particle size distribution of
unburned carbon particles of Vietnamese fly ash was determined by using wet sieve
analysis method and the amount of carbon retained in each size range is also
measured by LOI test. Vietnamese fly ash was sieved into different sizes: #30, 50,
100, 200 and 325. Particle size distribution of the fly ash measuring by wet sieving
method was conducted by calculating the weight percentage of fly ash retained on the
sieve. Size distribution of unburned carbon of Vietnamese fly ash of each sieve was
measured by calculating the weight percentage of carbon burnt out at 950°C. The
grinding process was repeated by adjusting the grinding conditions such as grinding
time, grinding repetitions and number of metal balls until the similar size distributions
of UC-FV and PAC were achieved. After that, the mix proportions of Mae-Moh fly
ash and PAC for making artificial high LOI fly ashes were calculated as shown in
Appendix B. Finally, the artificial high LOI fly ashes were then made, by mixing the
selected PAC with the low LOI fly ash from Mae-Moh power plant. The designated
%LOI of fly ashes were 0%, 6%, 12%, 18% and 25%.
Ref. code: 25605722040416SAT
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Figure 3.3 Planetary ball mill
Figure 3.4 Grinding process of powdered activated carbon (PAC)
Check size distribution of
UC-FV
(Reference)
Grind the Activated Carbon (AC)
Into PAC
Check Size Distribution of PAC
With UC-FV
Similar Finish
Much
Different
Ref. code: 25605722040416SAT
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Basic properties of
Artificial high LOI fly ash
- Loss on ignition
- Specific gravity
- Moisture content
- Blaine fineness
- Water retainability
-Water requirement
Clarification
Slump
Compressive strength
Slump model
Porosity
SEM
Micro hardness
Experimental Program
Basic and mechanical properties of
high LOI fly ash concrete
Durability of
High LOI fly ash concrete
Carbonation
Rapid Chloride Penetration Test
Shrinkage
Figure 3.5 Schematic outline of this study
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3.4 Experimental Methodology
This section describes details of test procedures, mix proportions and specimen
preparation for each experiment conducted in this study. The research scheme is
shown in Figure 3.5. The experiments include basic properties of artificial high LOI
fly ashes, basic and mechanical properties of the high LOI fly ash concrete. Some
durability properties of high LOI fly ash paste and concrete were also investigated.
Moreover, microstructure of high LOI fly ash concrete was also studied.
3.4.1 Properties of artificial high LOI fly ash
After all the artificial high LOI fly ashes had been made, the basic properties
such as LOI test, moisture content, specific gravity, Blaine fineness, particle size
distribution, water retainability and water requirement were tested.
3.4.1.1 Loss on Ignition
LOI test was carried out according to ASTM D7348 [34]. The apparatus for
LOI test are shown in Figures 3.6a to 3.6d. Place the samples for LOI test without
cover into preheated drying oven (104 to 110°C). Close the oven and heat for 1h to
eliminate the moisture. After that, remove the samples and cover immediately, allow
to cool off to ambient temperature in a desiccator. After the samples has cool down.
Place approximately 1 g of combustion residue into a pre-weighed crucible and weigh
the test specimen to the nearest 0.1 mg. Place the crucibles with the test specimen,
without a cover, into the cold furnace. Raise the temperature of the furnace at a rate
such that the furnace temperature reaches 450 to 500°C at the end of first hour and
950°C at the end of the second hour. Maintain the temperature for an additional two
hours or until the combustion residue test specimens reach a constant mass.
Calculate the percentage of loss on ignition to the nearest 0.1, as follows:
LOI, % =
A
B × 100 (3.1)
where :
A = loss in mass between 105°C and 950 °C
B = mass of moisture-free sample used
Ref. code: 25605722040416SAT
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a) Crucibles b) Balance
c) Oven d) Muffle furnace
Figure 3.6 Apparatus for LOI test
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3.4.1.2 Water retainability
Water retainability of a powder material is the water restricted by the powder
material, which includes water absorbed in the powder and that retained on its
surface. Tangtermsirikul and Kitticharoeniat [59] introduced an easy method for
estimating the water retainability of powder materials by finding a point of lowest
water to powder material ratio by weight that initiates slump of paste using a mini-
slump test (see Figure 3.7).
A metal mold, in the form of a frustum of a cone with dimensions as follows:
403 mm inside diameter at the top, 903 mm inside diameter at the bottom and 753
mm in height, and a metal tamper, weighing 34015 g and having a flat circular
tamping face 253 mm in diameter, are used in the mini slump test.
The test was first started by mixing the powder paste with a guessed value of
water to powder material ratio starting from a low ratio so that the mixture has no
slump. The mixture, approximately one third of the volume of the mold, is placed in
the mold and tamped 25 times with the tamper. The other two portions of the mixture
are placed and tamped until the mold is full. The excess is struck off and the mold is
immediately removed by raising it carefully in the vertical direction. The slump of the
mixture is measured. The entire process is repeated by increasing the water to powder
material ratio until slump is initiated. The water to powder material ratio, which
initiates slump, is the water retainability coefficient (β) of that powder material.
Figure 3.7 Mini slump test
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3.4.2 Basic and mechanical properties of high LOI fly ash concrete
The designation of mix proportion is labeled with the following nomenclature
(see Figure 3.8). W represents water to binder ratio of a mixture. W40 is water to
binder ratio of 0.4. OPC is cement only mixture (Ordinary Portland Cement type I).
FM is the mixture containing Mae-Moh fly ash. The number behind the letter FM
represents an approximate %LOI of the fly ash, which in this experiment ranges
approximately from 0.77% to 6, 12, 18 and 25%. r20 is the replacement percentage of
fly ash of 20%.
W40 OPC FM 12 r20
Figure 3.8 Mixture designation nomenclature
3.4.2.1 Slump
In order to investigate the effect of high LOI fly ash on workability of fresh
concrete, slump test was conducted according to the ASTM C143 [60]. The apparatus
for slump test is shown in Figure 3.9. After finishing concrete mixing, slump of the
fresh concrete was instantly measured and recorded as initial slump. In this study,
slump of concrete with high LOI fly ash, having %LOI of 0, 6, 12, 18 and 25%, were
tested in two w/b, which are 0.4 and 0.5. The details of all mix proportions for slump
test are shown in Table 3.4.
Water to binder
ratio LOI percentage of
fly ash
Containing fly ash Replacement
percentage
Ref. code: 25605722040416SAT
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Table 3.4 Mix proportions of concrete for slump test
Figure 3.9 Apparatus for slump test
kg kg kg kg kg
1 W40OPC 1.4 - 450.48 0.00 742.62 1075.62 180.19
2 W40FM0r20 1.4 20 347.31 86.83 742.62 1075.62 173.65
3 W40FM6r20 1.4 20 347.31 86.83 742.62 1075.62 173.65
4 W40FM12r20 1.4 20 347.31 86.83 742.62 1075.62 173.65
5 W40FM18r20 1.4 20 347.31 86.83 742.62 1075.62 173.65
6 W40FM25r20 1.4 20 347.31 86.83 742.62 1075.62 173.65
7 W40FM0r40 1.4 40 251.36 167.58 742.62 1075.62 167.58
8 W40FM6r40 1.4 40 251.36 167.58 742.62 1075.62 167.58
9 W40FM12r40 1.4 40 251.36 167.58 742.62 1075.62 167.58
10 W40FM18r40 1.4 40 251.36 167.58 742.62 1075.62 167.58
11 W40FM25r40 1.4 40 251.36 167.58 742.62 1075.62 167.58
12 W50OPC 1.4 - 395.37 0.00 742.62 1075.62 197.69
13 W50FM0r20 1.4 20 306.18 76.55 742.62 1075.62 191.36
14 W50FM6r20 1.4 20 306.18 76.55 742.62 1075.62 191.36
15 W50FM12r20 1.4 20 306.18 76.55 742.62 1075.62 191.36
16 W50FM18r20 1.4 20 306.18 76.55 742.62 1075.62 191.36
17 W50FM25r20 1.4 20 306.18 76.55 742.62 1075.62 191.36
18 W50FM0r40 1.4 40 222.52 148.35 742.62 1075.62 185.43
19 W50FM6r40 1.4 40 222.52 148.35 742.62 1075.62 185.43
20 W50FM12r40 1.4 40 222.52 148.35 742.62 1075.62 185.43
21 W50FM18r40 1.4 40 222.52 148.35 742.62 1075.62 185.43
22 W50FM25r40 1.4 40 222.52 148.35 742.62 1075.62 185.43
No. Mix ID γFly ash,
%
Proportions of concrete per 1 m3,
Portland
cement type Ifly ashes sand lime stone water
Ref. code: 25605722040416SAT
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3.4.2.2 Compressive strength
To investigate the effect of high LOI fly ash on compressive strength of
concrete, the compressive strength test was conducted in 3 different cases, which are
controlled water to binder ratio, controlled slump by using superplasticizer and
controlled slump by the adjustment of water. Mix proportions of high LOI fly ash
concrete for all cases are shown in Table 3.5. Water to binder ratios of 0.4 and 0.5
were used for the controlled water to binder ratio condition. For controlled slump
conditions, slump of concrete mixture was controlled at 8.5 ± 1 cm for both cases of
using type F naphthalene based superplasticizer and the adjustment of water. Fly
ashes with %LOI of 0, 6, 12, 18 and 25% were used to partially replace cement at
20% and 40% by weight. Moreover, different types of curing, which are water-cured
(WC) and air-cured (AC) conditions, were used to investigate the effect of internal
curing of concrete containing high LOI fly ash.
Cube concrete specimens with dimensions of 100x100x100 mm were used for
compressive strength test. Figure 3.10 shows the molds used to cast the compressive
strength test specimens. Three specimens were prepared for each mixture to obtain the
average compressive strength. Immediately after completion of molding, plastic
sheets were used to cover the top surface of specimens to prevent the moisture loss to
the environment. The specimens were demolded 24 hours after casting and exposed to
the two different curing conditions. All air-cured specimens were kept in a room with
temperature of 28 1C and RH of 75 5%. Compressive strength test was carried
out at the ages of 3, 7, 28 and 91 days by the compressive strength test machine (see
Figure 3.11).
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Figure 3.10 Cube molds having size of 10x10x10 cm for casting concrete
Figure 3.11 Compressive strength test machine
Ref. code: 25605722040416SAT
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Table 3.5 Mix proportions of concrete for compressive strength test.
% kg kg kg kg kg cc cm
1 W40OPC 0.40 - 450.48 0.00 742.62 1075.62 180.19 - 4.8
2 W40FM0r20 0.40 20 347.31 86.83 742.62 1075.62 173.65 - 7.4
3 W40FM6r20 0.40 20 347.31 86.83 742.62 1075.62 173.65 - 4.6
4 W40FM12r20 0.40 20 347.31 86.83 742.62 1075.62 173.65 - 3.6
5 W40FM18r20 0.40 20 347.31 86.83 742.62 1075.62 173.65 - 3.4
6 W40FM25r20 0.40 20 347.31 86.83 742.62 1075.62 173.65 - 1.7
7 W40FM0r40 0.40 40 251.36 167.58 742.62 1075.62 167.58 - 9.0
8 W40FM6r40 0.40 40 251.36 167.58 742.62 1075.62 167.58 - 6.5
9 W40FM12r40 0.40 40 251.36 167.58 742.62 1075.62 167.58 - 4.0
10 W40FM18r40 0.40 40 251.36 167.58 742.62 1075.62 167.58 - 2.5
11 W40FM25r40 0.40 40 251.36 167.58 742.62 1075.62 167.58 - 1.0
12 W50OPC 0.50 - 395.37 0.00 742.62 1075.62 197.69 - 13.0
13 W50FM0r20 0.50 20 306.18 76.55 742.62 1075.62 191.36 - 17.0
14 W50FM6r20 0.50 20 306.18 76.55 742.62 1075.62 191.36 - 15.0
15 W50FM12r20 0.50 20 306.18 76.55 742.62 1075.62 191.36 - 13.5
16 W50FM18r20 0.50 20 306.18 76.55 742.62 1075.62 191.36 - 11.5
17 W50FM25r20 0.50 20 306.18 76.55 742.62 1075.62 191.36 - 9.5
18 W50FM0r40 0.50 40 222.52 148.35 742.62 1075.62 185.43 - 20.5
19 W50FM6r40 0.50 40 222.52 148.35 742.62 1075.62 185.43 - 17.5
20 W50FM12r40 0.50 40 222.52 148.35 742.62 1075.62 185.43 - 15.5
21 W50FM18r40 0.50 40 222.52 148.35 742.62 1075.62 185.43 - 12.0
22 W50FM25r40 0.50 40 222.52 148.35 742.62 1075.62 185.43 - 8.5
23 W40OPC 0.40 - 450.48 0.00 742.62 1075.62 180.19 1441.53 8.0
24 W40FM0r20 0.40 20 347.31 86.83 742.62 1075.62 173.65 0.00 8.5
25 W40FM6r20 0.40 20 347.31 86.83 742.62 1075.62 173.65 651.21 8.2
26 W40FM12r20 0.40 20 347.31 86.83 742.62 1075.62 173.65 1215.58 7.8
27 W40FM18r20 0.40 20 347.31 86.83 742.62 1075.62 173.65 1736.55 8.0
28 W40FM25r20 0.40 20 347.31 86.83 742.62 1075.62 173.65 2257.51 7.6
29 W40FM0r20 0.40 20 347.31 86.83 742.62 1075.62 173.65 - 8.2
30 W40FM6r20 0.44 20 329.60 82.40 742.62 1075.62 181.28 - 8.0
31 W40FM12r20 0.46 20 321.41 80.35 742.62 1075.62 184.81 - 8.0
tested
slump
Case.1 controlled water to binder ratio
%r
fly
ash
Proportions of concrete per 1 m3
Case.2 controlled slump at 8.5 cm by using super plasticizer
Mix IDNo. w/bsuper
plasticizer
Case.3 controlled slump at 8.5 cm by adjusment of water
Portland
cement
type I
fly ashes sand lime stone water
Ref. code: 25605722040416SAT
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3.4.3 Durability of high LOI fly ash concrete
3.4.3.1 Autogenous shrinkage
The purpose of this experiment is to investigate the effect of high LOI fly ash
on autogenous shrinkage. Low to high LOI fly ashes with various %LOI of 0, 6, 12
and 18% were used to replace cement at 20%, by weight. Autogenous shrinkage of
cement and fly ash pastes were evaluated at w/b ratios of 0.25 and 0.4. Details of the
mix proportions are shown in Table 3.6. Paste specimens with dimensions of
25x25x285 mm were used. Figure 3.12 shows the molds used to cast shrinkage test
specimens. A total of 3 specimens were prepared for each mixture. Immediately after
completion of molding specimens, plastic sheets were used to cover the top surface of
specimens to avoid moisture loss to environment. After casting, the specimens were
kept in a controlled environment of 281C. Specimens were demolded at 24 hours
after casting and all of them were sealed by paraffin for the first layer. For the second
layer, specimens were wrapped by plastic sheets. Aluminum foil sheets were used as
the third layer. Figure 3.13 shows the final image of autogenous shrinkage specimens
after the preparation was finished. After that, the Initial length measurement using the
length comparator (Figure 3.14), were then taken on each specimen. The specimens
were kept in the controlled environment of 281C and 755% RH throughout the
experiment. The length change was measured daily for the first two weeks after
demolding and then once a week as the shrinkage rate are stabilized with time. The
autogenous shrinkage measurement was conducted for 91 days.
Figure 3.12 Bar molds for autogenous and total shrinkage test
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Figure 3.13 Autogenous shrinkage paste specimens
Figure 3.14 The length comparator used for measuring the expansion of
bar specimen
Ref. code: 25605722040416SAT
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3.4.3.2 Total shrinkage
Total shrinkage is mainly consisted of drying shrinkage and some amount of
autogenous shrinkage. The paste specimens for total shrinkage were prepared with the
same size and mix proportions of autogenous shrinakage. Three specimens were
prepared for each mixture. After completion of molding specimens, plastic sheets
were used to cover the top surface of specimens to avoid moisture loss. Specimens
were placed in a controlled environment of 281C and 755 RH. Specimens were
demolded at 24 hours after casting. All specimens were kept in the same controlled
environment as the autogenous shrinkage specimens (see Figure 3.15). The length
change of specimens was measured by using the length comparator (see Figure 3.14).
The length change was measured daily for the first two weeks after demolding and the
frequency of measurement was once a week as the shrinkage rate is gradually
stabilized with time. The total shrinkage measurement was conducted for 91 days.
Figure 3.15 Bar specimens for total shrinkage test
Ref. code: 25605722040416SAT
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Table 3.6 Mix proportions of pastes for autogenous shrinkage and total shrinkage
test.
3.4.3.3 Carbonation
Carbonation depth of cement-only concrete and fly ash concrete having
various %LOI ranges from 0 to 25% were tested in order to investigate the effect of
high LOI fly ash on carbonation resistance of concrete. Fly ash replacement was 20%.
Details of all mix proportions for carbonation test are presented in Table 3.7. The
effect of high LOI fly ash on carbonation was also tested at different water to binder
ratios of 0.4 and 0.5.
Cube concrete specimens having size of 100x100x100 mm were cast and
demolded at 24 hours after casting. Two curing conditions, which are water-cured and
air-cured conditions, were used to cure the concrete specimens for 28 days before
exposing to carbonation. In this study, accelerated carbonation test was selected in
order to shorten the test period. The CO2 subjection environment was controlled such
that the CO2 concentration, the temperature and the relative humidity were 4%
(40,000 ppm), 40±2°C and 55±5%, respectively. After CO2 subjection for 28 and 56
days, specimens were split into half and cleaned. The depth of carbonation was
determined by spraying 1% of phenolphthalein in the solution of 70% ethyl alcohol
FM0 FM6 FM12 FM18
1 W25OPC - 1.00 - - - - 0.25
2 W25FM0r20 20 0.80 0.20 - - - 0.25
3 W25FM6r20 20 0.80 - 0.20 - - 0.25
4 W25FM12r20 20 0.80 - - 0.20 - 0.25
5 W25FM18r20 20 0.80 - - - 0.20 0.25
6 W40OPC - 1.00 - - - - 0.25
7 W40FM0r20 20 0.80 0.20 - - - 0.25
8 W40FM6r20 20 0.80 - 0.20 - - 0.25
9 W40FM12r20 20 0.80 - - 0.20 - 0.25
10 W40FM18r20 20 0.80 - - - 0.20 0.25
fly ashesNo. Mix ID Fly ash, %
Mix proportion(ratio by weight)
Portland
cement type Iw/b
Ref. code: 25605722040416SAT
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[61] on a freshly broken surface. The phenolphthalein solution is colorless but its
color could changes to purple when pH of the concrete specimen is higher than the
range of approximately 9. Therefore, when the solution is sprayed on a broken
concrete surface, the carbonated portion undergoes no color change and the non-
carbonated portion changes to purple (see Figure 3.16). The depth of carbonation is
defined as the thickness of carbonated portion. The carbonation depth was taken as
the average of 12 carbonation depth readings measured from four sides of the broken
surface of the specimens.
Figure 3.16 Specimens after spraying phenolphthalein solution
Ref. code: 25605722040416SAT
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3.4.3.4 Rapid Chloride Penetration Test (RCPT)
In this study, chloride resistance was observed in terms of chloride
permissibility. To study the chloride resistance of high LOI fly ash concrete, the
chloride permissibility of cement-only concrete and fly ash concrete having various
%LOI ranges from 0 to 25% were tested by mean of rapid chloride penetration test
(RCPT). Cylinder molds (Figure 3.17) having diameter and height of 100 mm and
200 mm, respectively, were used to cast concrete. After demolding, all the specimens
were cured in the water until the test ages. The RCPT was conducted at the age of 28,
56 and 91 days. At the test ages, each specimen was cut into 3 slices, having a
thickness of 51 ± 3 mm (Figure 3.18). The samples preparation and procedures for
RCPT were performed according to ASTM C1202 [62]. The current was read and
recorded every 30 min using a data logger (Figure. 3.19). The effect of high LOI fly
ash on chloride resistance of concrete was also tested at different water to binder
ratios of 0.4 and 0.5. Fly ash replacement percentage was 20%. Details of all mix
proportions for RCPT test are shown in Table 3.7.
Figure 3.17 Cylinder molds
Ref. code: 25605722040416SAT
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Figure 3.18 A slice of RCPT specimen
Figure 3.19 Apparatus for Rapid Chloride Penetration Test
Ref. code: 25605722040416SAT
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Table 3.7 Mix proportions of concrete for carbonation and RCPT test.
kg kg kg kg kg
1 W40OPC 0.4 - 450.48 0.00 742.62 1075.62 180.19
2 W40FM0r20 0.4 20 347.31 86.83 742.62 1075.62 173.65
3 W40FM6r20 0.4 20 347.31 86.83 742.62 1075.62 173.65
4 W40FM12r20 0.4 20 347.31 86.83 742.62 1075.62 173.65
5 W40FM18r20 0.4 20 347.31 86.83 742.62 1075.62 173.65
6 W40FM25r20 0.4 20 347.31 86.83 742.62 1075.62 173.65
7 W40FM0r40 0.4 40 251.36 167.58 742.62 1075.62 167.58
8 W40FM6r40 0.4 40 251.36 167.58 742.62 1075.62 167.58
9 W40FM12r40 0.4 40 251.36 167.58 742.62 1075.62 167.58
10 W40FM18r40 0.4 40 251.36 167.58 742.62 1075.62 167.58
11 W40FM25r40 0.4 40 251.36 167.58 742.62 1075.62 167.58
12 W50OPC 0.5 - 395.37 0.00 742.62 1075.62 197.69
13 W50FM0r20 0.5 20 306.18 76.55 742.62 1075.62 191.36
14 W50FM6r20 0.5 20 306.18 76.55 742.62 1075.62 191.36
15 W50FM12r20 0.5 20 306.18 76.55 742.62 1075.62 191.36
16 W50FM18r20 0.5 20 306.18 76.55 742.62 1075.62 191.36
17 W50FM25r20 0.5 20 306.18 76.55 742.62 1075.62 191.36
18 W50FM0r40 0.5 40 222.52 148.35 742.62 1075.62 185.43
19 W50FM6r40 0.5 40 222.52 148.35 742.62 1075.62 185.43
20 W50FM12r40 0.5 40 222.52 148.35 742.62 1075.62 185.43
21 W50FM18r40 0.5 40 222.52 148.35 742.62 1075.62 185.43
22 W50FM25r40 0.5 40 222.52 148.35 742.62 1075.62 185.43
No. Mix ID w/bFly ash,
%
Proportions of concrete per 1 m3
fly ashes sand lime stone waterPortland
cement
type I
Ref. code: 25605722040416SAT
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3.4.4 Microstructure of high LOI fly ash concrete
3.4.4.1 Porosity of fly ash mortar and concrete
Porosity of mortars and concrete containing low and high LOI fly ash, having
%LOI of 0.77, 6 and 12% were tested according to ASTM C642 [63]. Cube
specimens having dimension of 50x50x50 mm were used to determine the porosity of
mortar and specimens having dimension of 60x60x100 mm were used to determine
the porosity of concrete. Two water-cured specimens were used per each mortar and
concrete mixture to obtain the average void value. The w/b of tested mixtures were
0.25 for fly ash mortar and 0.4 for fly ash concrete. The porosity determination in this
study was carried out at the age of 3 days for mortar and 28 days for concrete.
3.4.4.2 Micro hardness
It has been found by some previous researches that the use of bottom ash or
other light weight aggregate, which are porous materials, form the formation of a hard
shell around their particles and significantly influences the mechanical properties of
the concrete [65-67]. Therefore, micro hardness test on high LOI fly ash concrete was
conducted, since high LOI fly ash is also a porous material.
Micro hardness test was carried out for W40FM0 and W40FM12 mixtures,
which are low w/b fly ash concrete (w/b=0.4) containing fly ashes with LOI of 0.77
and 12%, respectively. Concrete specimens having size of 100x100x100 mm were
cast and cured in water for 28 days. After that they were cut into small cube
specimens having dimension of 10x10x10 mm by a diamond cutter. The small
concrete cubes were then submerged in acetone solution for 24 hours in order to stop
the hydration reaction of cement paste. After that, the specimens were dried, by
keeping it in the oven at 55°C for another 24 hours. Finally, the dried specimens were
put into a vacuum container for 12 hours.
Three concrete cubes having size of 10x10x10 mm were put into a mold (Fig
3.20). Choose the test surface that contains large paste area in order to investigate
micro hardness around fly ash and carbon particles and make sure that the chosen test
surface are attached to the bottom of the mold. The resin solution was made from
Epofix Resin and EpoFix hardener with the ratio of 1:8 by volume. The prepared resin
solution was then poured into the molds under the pressure of 90 kPa for 1 hour. The
Cito Vac instrument was used in order to eliminate the air inside the samples and to
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make the resin solution deeply penetrate into the samples. Next, all molds were kept
in the oven at 50°C and demolded after 24h. After that, the surface of the specimens
and resin were together smoothened by polishing with sand papers No. 120, 220, 500,
800 and 1200, respectively. The final specimen after polishing is shown in Figure
3.21.
In this study, the Vickers hardness test was conducted, following ASTM
C1326 and C1327. In this method, Vickers indenter, made from diamond of specific
geometry, was pressed into the test specimen surface under an applied force of 150gf
using a test machine specifically designed for such work, as seen in Figure 3.22. The
Vickers hardness number is based upon the force divided by the surface area of the
indentation. It is assumed that elastic recovery does not occur when the indenter is
removed. In this study, hardness values at distances of 20 μm to 250 μm from the
boundary of the unburned carbon and fly ash particles were measured.
Figure 3.20 Mold and cube concrete Figure 3.21 Concrete cubes inside resin
specimens after polishing
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Figure 3.22 Vickers hardness test apparatus
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Chapter 4
Results of Basic Properties of High LOI Fly Ash
4.1 General
Artificial high LOI fly ashes were made by mixing low LOI fly ash from Mae-
Moh power plant with a powdered activated carbon (PAC). Chemical compositions of
cement, fly ash and PACs were tested by XRF. In order to make artificial high LOI
fly ash, the information about morphology and surface texture of unburned carbon
particles in fly ash are crucial for making decision on which PACs will be use.
Therefore, Microscopic studies of low and high LOI fly ashes and PACs, were carried
out by Scanning Electron Microscope (SEM). The elemental compositions of fly ash
particles were also tested by Energy Dispersive X-ray (EDX).
4.2 Morphology of fly ashes and powdered activated carbons (PACs)
4.2.1 Morphology of fly ashes with various %LOI
SEM pictures of Mae-Moh fly ash with low LOI content (Figure 4.1) show that
most of its particles are small and big spheres. Some particles with porous and
irregular shape were observed in BLCP fly ash (Figure 4.2), which has %LOI of
5.36%. When %LOI is 18.04%, in case of Vietnamese fly ash (Figure 4.3), there were
plenty of the irregular and porous particles mixing with the fine round spheres.
Majority of the irregular particles, often found in high LOI fly ashes, are believed to
be the unburned carbon particles. Therefore, the EDX test was carried out on some of
the irregular particles. The EDX result of particle #1, as illustrated in Figure 4.4,
demonstrates the high amount of carbon percentage of the particular area tested on
that particle. Hence, it can be said that it is an unburned carbon particle.
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(a) x200
(b) x1000
Figure 4.1 SEM pictures of a low LOI fly ash (LOI= 0.77%)
from Mae-Moh power station, Thailand
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(a) x200
(b) x1000
Figure 4.2 SEM pictures of a high LOI fly ash (LOI = 5.36%)
from BLCP power station, Thailand
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(a) x200
(b) x1000
Figure 4.3 SEM pictures of a high LOI fly ash (LOI=18.04%)
from Vietnam
#1
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Figure 4.4 EDX result of particle #1 (see Figure 4.3a), Vietnamese fly ash
4.2.2 Morphology of Powdered Activated Carbons (PACs)
The PACs in this research were from 3 available sources of activated carbon
in Thailand, which are activated carbon produced from coconut shell, bituminous coal
and wood. The carbon content, tested by LOI test, of the 3 PACs were 85.28%,
86.18% and 80.37% respectively. PAC selection was considered based only on their
physical properties, especially the particle shape by SEM. This is because the
unburned carbon particles are the non-reactive portion of fly ash [68]. Therefore, its
physical properties have more influences on properties of concrete when compared to
its chemical composition. Activated carbon was in the form of granular and powdered
activated carbon. The granular activated carbon were ground to powdered activated
carbon before SEM test. Figures 4.3a to 4.3c show particle shapes of PAC-CS, PAC-
BC and PAC-W by SEM, respectively. Rough texture of PAC-BC and PAC-W were
similar to that of the unburned carbon particles of Vietnamese fly ash (UC-FV) while
PAC-CS has quite smooth surface. However, the shape and pore structure of PAC-W
were totally different from PAC-CS and UC-FV. Therefore, PAC-BC was selected for
preparing artificial high LOI fly ash in this experiment.
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(a) PAC-CS
(b) PAC-BC
(c) PAC-W
Figure 4.5 SEM pictures of Powdered Activated Carbons (PACs)
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4.3 Properties of artificial high LOI fly ash
The selected activated carbon, which is the one produced from Bituminous
coal (PAC-BC), was ground to have similar particle size distribution to the unburned
carbon particles in the Vietnamese fly ash (Figure 4.6). After that the ground activated
carbon or powdered activated carbon (PAC-BC) was thoroughly mixed with Mae-
Moh fly ash by a mixing machine in order to increase LOI of fly ash from 0.77% to
approximately 6%, 12%, 18% and 25%. In this research, these new fly ashes were
called the artificial high LOI fly ashes. Figures 4.7a and 4.7b compare the SEM
images of the real high LOI fly ash from Vietnam with the produced artificial high
LOI fly ash (both having %LOI approximately of 18%). After all the artificial high
LOI fly ashes had been prepared, their basic properties were tested.
Figure 4.6 Particle size distributions of UC-FV and PAC-BC
0
20
40
60
80
100
0.01 0.1 1 10 100 1000
Cum
ula
tive
Pas
sing (
%)
Sieve Size (micron)
Unburned Carbon in Vietnamese fly ash(UC-FV)
Powdered Activated Carbon (PAC-BC)
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a) Real high LOI fly ash from Vietnam (LOI=18.04%)
b) Artificial high LOI fly ash (LOI=18.41%)
Figure 4.7 SEM pictures of real and artificial high LOI fly ashes
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4.3.1 Basic properties of fly ash
It is noted that the actual %LOI in the prepared fly ashes for the tests in this
study are not exactly 0%, 6%, 12%, 18% and 25% but are the values listed in Table
4.1. The values in Table 4.1 are the actually tested LOI of the prepare fly ashes. The
results of tested basic properties of artificial high LOI fly ashes containing various
%LOI ranging from 0.77% to approximately 25% are shown in Table 4.2. When
%LOI of fly ash increases from 0.77% to 25.37%, moisture content also increases
from 0.29 to 2.02. However, the moisture content of all fly ashes, are still lower than
that of the allowable limit in the standard specification, which ASTM C618 limits the
maximum moisture content of fly ash at 3%. Surface area of fly ashes, which can be
approximately determined by Blaine fineness method, increases from 2837 to 3561
cm2/g as the %LOI of fly ash increases from 0.77% to 25.37%. The Specific gravity
of fly ashes decreases from 2.21 to 2.02, showing that high LOI fly ash is lighter than
low LOI fly ash.
Table 4.1 Actual tested %LOI in the prepared fly ashes
Tested fly ash Actual %LOI
FM0 0.77 %
FM6 6.22 %
FM12 12.37 %
FM18 18.41 %
FM25 25.37 %
Table 4.2 Moisture content, specific gravity and Blaine fineness of fly ashes with
various %LOI
Artificial high
LOI Fly ash ID
Moisture
(%)
Specific
gravity
Blaine fineness
(cm2/g)
FM0 0.29 2.21 2837
FM6 0.50 2.16 3038
FM12 1.26 2.12 3164
FM18 1.77 2.07 3388
FM25 2.02 2.02 3561
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4.3.2 Particle size distribution
Particle size distribution results of cement, artificial high LOI fly ash with
various %LOI and PAC produced from bituminous coal were tested by Laser
diffraction technique (see Figure 4.8). The result shows that OPC has the finest
particle size distribution whereas the particle size of PAC is the coarsest. Fly ash with
%LOI of 0.77% has finer particle size distribution than those of high LOI fly ashes.
Particle size distribution of fly ash becomes coarser as the %LOI of fly ash increases.
Nevertheless, since the specific surface area of high LOI fly ash is higher than the low
LOI fly ash while it is coarser, this result is one of the evidences indicating that high
LOI fly ash definitely has a more porous structure.
Figure 4.8 Particle size distributions of cement, fly ashes with various %LOI and
PAC produced from bituminous coal
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4.3.3 Water retainability
Figure 4.9 shows the result of water retainability of fly ashes, which was
tested according to the test method proposed by Tangtermsirikul and Kitticharoeniat
[60] The water retainability of fly ashes gradually increase from 0.18 to 0.35 with the
increase of %LOI of fly ashes from 0.77 to 25.37%. The water retainabilityof fly
ashes having %LOI equal to or higher than 12% were greater than that of OPC. Water
retainability of powder depends on many parameters, such as porosity, environment
temperature, surface condition, shape and size distribution of powder. Considering
physical properties, it was found that restricted water on granular powder is greater
than spherical powder.
Figure 4.9 Water retainability coefficients of fly ashes with various %LOI
0.18
0.22
0.25
0.30
0.35
OPC=0.23
0.00
0.10
0.20
0.30
0.40
0 6 12 18 25
Wat
er r
etai
nab
ilit
y c
oef
fici
ent
LOI of fly ash, %
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4.3.4 Water requirement
Water requirement of mortars containing fly ashes with various %LOI of
approximately 0.77, 12, 18 and 25% are shown in Figure 4.10. In this case, the fly
ash replacement percentage of 20% was used as a cement replacement in the
mixtures. The result shows that only fly ash with LOI of 0.77% requires less water
requirement than the mortar incorporating only cement. It can be obviously seen that
as %LOI of fly ash increases from 0.77 to 25.37%, water requirement of mortars also
gradually increases from 97.12 to 104.39%.
Figure 4.10 Water requirement of mortars containing fly ashes with various %LOI
100.00
97.12
100.68
102.78 104.39
80
85
90
95
100
105
110
OPC
FMr2
0
FM12
r20
FM18
r20
FM25
r20
Wat
er r
equir
emen
t, %
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Chapter 5
Results and Clarifications of Slump
5.1 Initial slump of concrete
The initial slump of concrete mixtures was tested at water to binder ratios of 0.4
and 0.5 (see Figures 5.1 and 5.2, respectively). Fly ashes having various %LOI were
used as a cement replacement at 20% and 40% (by weight). It can be obviously seen
from the results that fly ash mixture with the lowest %LOI (LOI= 0.77%) has the
highest slump. In case of w/b of 0.4 (see Figure 5.1), when %LOI of fly ash increases
from 0.77 to 25.37%, slump of fly ash concrete gradually decreases from 7.4 cm to
1.7 cm (%r=20%) and 9.0 cm to 1.0 cm (%r=40%). For mixtures of w/b of 0.5 (see
Figure 5.2), when %LOI of fly ash increases from 0.77 to 25.37%, slump of fly ash
concrete also gradually decreases from 17.0 cm to 9.5 cm (%r=20%) and 9.0 cm to
1.0 cm (%r=40%).
It can be said that the higher the LOI percentage of fly ash is, the more the
slump of fly ash concrete is reduced for all w/b ratios and fly ash replacement
percentages, due to the irregular shape and porous characteristic of the high LOI fly
ash particles. However, slump of mixtures containing fly ash having %LOI lower or
equal to 6% in case of w/b ratio of 0.4 (see Figure 5.1) and 12% in case of w/b ratio
of 0.5 (see Figure 5.2), can be higher or equal to the slump of OPC mixtures when fly
ash were replaced at 20%. These results correspond to the limitation of %LOI in
ASTM or many other countries’ standards, which mostly limit the maximum %LOI of
fly ash using in concrete at about 6%.
Increasing fly ash content in the mixtures from 20% to 40% replacement greatly
improves the workability of fresh concrete for mixtures containing fly ash that has
%LOI lower or equal to 6% (in case of w/b ratio = 0.4) and 12% (in case of w/b ratio
= 0.5). As the slump of fly ash concrete gradually decreases with the increase of
%LOI of fly ash, increasing the replacement percentage of fly ash that has %LOI
greater than 12% in the mixtures adversely affects the slump by decreasing the slump
of concrete even more. It can be observed from Figures 5.1 and 5.2 that the lines of
fly ash replacements of 20% and 40% intersect at a certain %LOI of the fly ash,
meaning that, using not too high LOI fly ashes, higher fly ash replacement offers
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better slump performance. On the other hand, when very high LOI fly ashes are used,
higher fly ash replacement can lead to a lower slump performance. This behavior will
be explained in the section 5.2.
Figure 5.1 Initial slump of concrete containing fly ashes with various %LOI
(w/b = 0.4)
Figure 5.2 Initial slump of concrete containing fly ashes with various %LOI
(w/b = 0.5)
OPC=4.8
0
2
4
6
8
10
0 6 12 18 25
Init
ial
Slu
mp (
cm)
LOI of fly ash, %
r20 r40
OPC=13
0
5
10
15
20
25
0 6 12 18 25
Init
ial
Slu
mp (
cm)
LOI of fly ash, %
r20 r40
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5.2 Clarification of slump behavior
It was found that the higher the LOI percentage of fly ash, the more slump of fly
ash concrete is reduced for all tested w/b ratios (0.4 and 0.5). Moreover, increasing fly
ash content in the mixtures from 20% to 40% replacement improves the workability
of fresh concrete for mixtures containing fly ash having %LOI lower or equal to 12%.
On the contrary, the slump of fly ash mixture, having %LOI higher than 12%,
gradually decrease with the increase of fly ash replacement percentage. This
phenomenon created the intersection between the lines of two replacement
percentages of fly ash. The reasons for the intersection of slump graphs discussing
before, were explained by adopting the slump prediction model, which describes the
relationship between the effect of water retainability and the lubrication effect of fly
ash. In this segment, slump prediction model [69] will be employed to explain the
slump behavior of the fly ash concrete.
5.2.1 Background of slump model
Model for predicting workability of fresh concrete was proposed by
Tangtermsirikul et al [69] are shown in Eq (5.1).
SL = α(Wfr − W0) (5.1)
where Wfr is volume of free water in the fresh concrete mixture (kg/m3 of concrete),
W0 is the minimum free water content required initiating slump (kg/m3 of concrete), α
is the slope of slump-free water content curve (cm/kg/m3 of concrete), and SL is
slump value of fresh concrete (cm).
5.2.1.1 Slope of slump-free water content curve (𝛂)
It was found that slopes of the slump-free water content curves increased with
the increase of ratio between paste volume and void content of compacted aggregate
phase (). It is noted here that some effect of aggregate properties are indirectly
considered by, such as gradation and aspect ratio. The ratio of paste volume to void
content of compacted aggregate phase is defined as:
γ =
Vp
Vvoid (5.2)
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where Vp is the volume of paste in the unit volume (1 m3) of fresh concrete and Vvoid
is the volume of void in the densely compacted total aggregate (fine and coarse
aggregate) in the unit bulk volume (1 m3) of aggregate. The volume of paste can be
derived as:
Vp = Vc + Vw + Vair + Vpow (5.3)
where Vc, Vw, Vair and Vpow are the volume of cement, water, air and other powder
materials, respectively, in a unit volume (1 m3) of concrete mixture.
The relationship between slope of slump-free water content curve () and
value of was found from the analysis of experimental data as shown in Eq. (5.4).
α = 3.57γ4 − 21.34γ3 + 46.74γ2 − 43.92γ + 14.94 (5.4)
5.2.1.2 Free water content in fresh concrete (Wfr)
Free water means the amount of water that is free, by any means, from being
restricted by all solid particles in the fresh concrete and can be obtained from unit
water content minus water retainability of powder materials and surface water
retainability of aggregates as:
Wfr = Wu − Wrp − Wra′ (5.5)
where Wu is the unit water content in the mixture (kg/m3 of concrete), Wrp is the
restricted water by powder materials (kg/m3 of concrete), and Wra′ is the restricted
water at the surface of aggregates (kg/m3 of concrete).
(1) Water retainability of powder materials (𝛃𝒑)
The total amount of restricted water by all powder materials can be
derived from the summation of the product between the weight of each
powder and its water retainability.
Wrp = ∑ β𝑝𝑖𝑤𝑝𝑖
𝑛
𝑖=1
(5.6)
where β𝑝𝑖 is the water retainability coefficient of powder material type i which
is obtained from the tested water retainability coefficient results in chapter 4,
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w𝑝𝑖 is the absolutely dried weight of powder material type I (kg/m3 of
concrete), n is total number of powder materials used in the concrete.
(2) Surface water retainability of aggregates (𝐖𝐫𝐚′ )
In mix design of concrete, unit water content does not include the
absorption of aggregates. So the restricted water in addition to the absorbed
water in the aggregate particles is considered here. The surface water
retainabilithy of aggregates can be expressed as:
Wra′ = βs
′ ws′ + βg′wg′ (5.7)
where , βs′ , βg′ are the surface water retainability coefficients (excluding
absorption) of fine and coarse aggregates, respectively, and ws′ , wg′ are
saturated surface dried weights of sand and gravel respectively (kg/m3 of
concrete).
(a) Water retainablity coefficient of aggregates (𝛃𝐚𝐠𝐠′)
It was assumed that the water retainability of aggregates depends
on irregularity and size of the particles so that specific surface area can
be considered an appropriate parameter. The derived surface water
retainability coefficient of aggregates including sand and gravel is as
follow.
βagg′ = 2 × 10−6(Sagg)0.9
(5.8)
where βagg′ is the surface water retainability coefficient (excluding
absorption) of aggregate (g/g of SSD aggregate) and Sagg is specific
surface area of aggregate (cm2/kg). in practice, the water retainability
of coarse aggregate can be neglected due to its small value when
compared to that of the fine aggregate.
(b) Determination of specific surface area of fine and coarse
aggregates
In this study, a calculation method was used to compute surface
area of aggregate by first assuming that the shape of aggregate particle is
spherical. The specific surface area of aggregate on spherical shape basis
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can be calculated from the gradation as expressed in the following
equation.
So =
6000
Dav × ρ (5.9)
Dav =
∑ D𝑖𝑀𝑖
∑ M𝑖 (5.10)
where S0 is the specific surface area of aggregate on spherical shape
basis (cm2/g), Dav is the average diameter of the aggregate particles
(cm), Di is the average dimension between the upper sieve and the sieve
i on which aggregate particles are retained (cm), Mi is the percentage of
retaining on the corresponding sieve of the aggregate group i, (%), and ρ
is the specific gravity of the aggregate.
Then angularity factor is applied to account for the irregularity of
the particles. As the result, the specific surface area of irregular
aggregate can be estimated by multiplying the angularity factor to the
specific surface area of the assumed spherical aggregate, that is
calculated from sieve analysis as:
Sg = ψg × Sgo (5.2)
Ss = ψs × Sso (5.3)
Where Ss and Sg are the specific surface area of irregular fine and coarse
aggregates, respectively (cm2/g). ψs and ψg are the angularity factors of
fine and coarse aggregates, respectively. Sso and Sgo are the specific
surface area of the assumed spherical fine and coarse aggregates,
respectively (cm2/g).
5.2.1.3 Minimum free water content required to initiate slump (Wo)
The interparticle surface forces vary with the numbers of feasible interparticle
contact among the solid particles, and particles with the larger surface are result in
more contacts. As the result, the interparticle surface forces can be considered to vary
with the surface area of the solid particles that have possibility to be in contact, which
is defined in this study as effective surface area (Seff, cm2/m3 of concrete). Then, the
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amount of water for balancing these interparticle surface forces (Wo) can be expressed
as a function of Seff.
It is well known that spherical fillers can reduce interparticular friction among
larger particles, i.e. cement-to-cement, cement-to-aggregate, and aggregate-to-
aggregate frictions. This effect is identified as lubrication effect. Lubrication is
thought to reduce friction and therefore Wo. The lubrication coefficient (L) was
introduced to account for lubrication effect of spherical-shape powder. The empirical
equation for Wo was derived as:
Wo = [8 × 10−5(Seff)0.70]/L (5.4)
1) Effective surface area of solid particles (𝐒𝐞𝐟𝐟)
The effective surface area of solid particles indicates the possible
contacts among the fine aggregates, coarse aggregate and powder. It was
derived as in the following equation.
Seff = Stagg + η(Spow) (5.5)
Spow = 1000 ∑ Spiwpi
n
i=1
(5.6)
Stagg = 1000(Ssws + Sgwg) (5.7)
where Stagg and Spow are surface area of total aggregates and total powder
materials in concrete, respectively (cm2/m3 of concrete) ws, wg, and wpi are the
saturated surface dried weight of fine aggregate coarse aggregate, and the
absolutely dried weight of powder material type I, respectively (kg/m3 of
concerete). Ss, Sg, and Spi are the specific surface area of fine aggregate,
coarse aggregate, and powder material type I, respectively (cm2/g). n is total
number of powder material used in the concrete. η is the effective contact area
ration indicating the ratio of surface area of powder material, which is
effectively contact around aggregates, which was derived as:
η = 0.026e−3×10−8(Stagg) (5.8)
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2) Lubrication coefficient (L)
The major parameters that affect this coefficient were considered to be
the ratio of specific surface area of powder to specific surface area of cement
and replacement ratio. This is because finer powders are more efficient than
coarser powders in lubrication, and more amount of powder is also more
effective. The shape factor was introduced to incorporate the effect of particle
shape on the lubrication effect by considering that granular particles will have
no lubrication effect whereas spherical particles will have perfect lubrication.
So, the equation for lubrication effect was derived as:
L = 1 + bRc(1.4 − φ) (5.9)
where b = −8.35r2 − 0.24r + 0.19 (5.10)
c = −15.6r2 + 6.0r + 0.5 (5.20)
where R is the ratio of specific surface area of powder to specific surface area
of cement, φ is angularity factor obtained from back calculation and r is
replacement ratio of fly ash.
5.2.2 Verification of initial slump of high LOI fly ash concrete
The tested slump results of fly ash concrete with various LOI percentages, water
to binder ratios and fly ash replacement percentages were compared with the
predicted slump calculated from the proposed model. Both the tested slump and
predicted slump values of fly ash concrete with w/b ratios of 0.4 and 0.5 are shown in
Tables 5.1 and 5.2, respectively. The tested initial slump results obtained from initial
slump test in section 5.1 are shown in Figures 5.1and 5.2 respectively. The predicted
slump results obtained from the slump model are shown in Figures 5.3 and 5.4, for
w/b of 0.4 and 0.5, respectively.
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Table 5.1 Tested and predicted slump results of fly ash concrete containing various
%LOI (w/b =0.4)
w/b %r
LOI, Tested Predicted Error
% (cm) (cm) cm %
0.4
20
0 7.4 5.2 2.2 29
6 4.6 4.4 0.2 4
12 3.6 3.8 -0.2 -5
18 3.4 2.8 0.6 18
25 1.7 1.7 0.0 -1
40
0 9.0 7.7 1.3 14
6 6.5 6.1 0.4 6
12 4.0 4.8 -0.8 -20
18 2.5 2.8 -0.3 -11
25 1.0 0.7 0.3 33
Table 5.2 Tested and predicted slump results of fly ash concrete containing various
%LOI (w/b =0.5)
w/b %r
LOI, Tested Predicted Error
% (cm) (cm) cm %
0.5
20
0 17.0 11.9 5.1 30
6 15.0 11.2 3.8 25
12 13.5 10.6 2.9 21
18 11.5 9.7 1.8 15
25 9.5 8.8 0.7 7
40
0 20.5 14.2 6.3 31
6 17.5 12.7 4.8 27
12 15.5 11.6 3.9 25
18 12.0 9.8 2.2 19
25 8.5 7.9 0.6 7
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The predicted slump results obtained from the slump model were quite
accurate, especially for the predicted slump of those high LOI fly ash mixtures. The
intersection between the lines of two replacement percentages of fly ash, which are
20% and 40%, were also obtained in the predicted slump graph (see Figures 5.3 and
5.4). The reason for these intersection points could be due to the opposite influences
of water retainability and lubrication effect of the high LOI fly ashes. As we can see
that the water retainability is involved in the amount of free water content (Wfr) of a
mixture as shown in equations (5.5) and (5.6). Lubrication effect is involved in the
minimum water content required to initiate the slump of fresh concrete (Wo) as shown
in equation (5.13). The water retainability and lubrication coefficients are shown in
Figures 5.5 and 5.6, respectively. The relationship between Wfr and Wo and %LOI of
fly ash are shown in Figure 5.7. It was found from Figures 5.5 to 5.7 that when LOI
increases, water retainability also increases causing lower free water content (Wfr) and
so lowering the slump of concrete. Lubrication effect helps to reduce the minimum
water content required to initiate slump (W0) and happens only on fly ash at low LOI,
because granular particles will have no lubrication effect whereas spherical particles
will have perfect lubrication. So, when %LOI of fly ash increases, the increase in
granular and porous particles of fly ash lowers its lubrication effect and finally
resulting in high W0. Higher W0 lowers free water of the mixture. Therefore,
increasing replacement percentage of high LOI fly ash will further decrease the slump
of concrete because of both the reduction of free water content (Wfr) due to the
increase in water retainability and the increasing of W0 due to the lowering of
lubrication effect of high LOI fly ash. More vigorous influence on slump when
increasing fly ash replacement percentage is on the reduction of free water (Wfr) due
to increase of %LOI as can be seen from Figure 5.7. Figure 5.7 shows that when
%LOI fly ash replacement is 40%, the slope of the Wfr curve becomes much steeper
when compared to that of the 20% fly ash replacement while the slopes of the W0
curves of both 20% and 40% fly ash replacements are not much different.
Ref. code: 25605722040416SAT
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Figure 5.3 Predicted slump of fly ash concrete with various %LOI
(w/b = 0.4)
Figure 5.4 Predicted slump of fly ash concrete with various %LOI
(w/b = 0.5)
0
2
4
6
8
10
0 6 12 18 25
Init
ial
Slu
mp (
cm)
LOI of fly ash, %
r20
r40
0
5
10
15
20
25
0 6 12 18 25
Init
ial
Slu
mp (
cm)
LOI of fly ash, %
r20
r40
Ref. code: 25605722040416SAT
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Figure 5.5 Water retainability coefficients of fly ashes
with various %LOI
Figure 5.6 Lubrication coefficients of fly ashes
with various %LOI
0.18
0.220.25
0.3
0.35
0.00
0.10
0.20
0.30
0.40
0 6 12 18 25
Wat
er r
etai
nab
ilit
y c
oef
fici
ent
%LOI of fly ash
1.145
1.150
1.155
1.160
1.165
1.170
1.175
0 6 12 18 25
Lub
rica
tion
coef
fici
ent
%LOI of fly ash
Ref. code: 25605722040416SAT
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Figure 5.7 Relationship between Wfr, W0 and %LOI of fly ash
(w/b =0.4)
0.0
10.0
20.0
30.0
40.0
50.0
60.0
70.0
0 6 12 18 25
Volu
me
of
free
wat
er (
Wfr)
and W
0
(kg/m
3)
LOI of fly ash, %
Wfr (r20) W0 (r20)
Wfr (r40) W0 (r40)
Ref. code: 25605722040416SAT
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Chapter 6
Results and Clarifications of Compressive Strength
6.1 General
Compressive strength of high LOI fly ash concrete were tested in controlled
slump and controlled water to binder ratio conditions. The effect of fly ash content
was also tested, by using 2 fly ash replacement percentages, which are 20% and 40%
by weight of the total binders. Moreover, different type of curing conditions, which
are water curing and air curing, were also used to test curing sensitivity of high LOI
fly ash concrete. Then, microstructure of high LOI fly ash concrete was investigated
in order to explain the compressive strength results.
6.2 Effect of high LOI fly ash on compressive strength of concrete
6.2.1 Controlled slump
This section presents the effect of high LOI fly ash on compressive strength of
concrete in controlled slump condition. Slump of concrete was controlled at 8.5 ± 1
cm by 2 methods, adjustment of water and use of type F naphthalene based
superplasticizer. Replacement percentage of fly ash was maintained at 20%. All
mixtures were cured in water until the test ages of 3, 7, 28, 91 days.
The compressive strength of fly ash concrete, in case of controlled slump by
adjustment of water (see Figure 6.1), gradually decreases with the increase of %LOI
of fly ash for all tested ages. In case of controlled slump by the use of superplasticizer
(Figure 6.2), when %LOI is increased up to 12%, compressive strength of fly ash
concrete at early-age tends to increase with the increase of %LOI of fly ash. Then it
gradually decreases with the increase of LOI when %LOI of fly ash is beyond 12%.
Long-term compressive strength of all high LOI fly ashes were comparable to low
LOI fly ash (LOI=0.77%). These results are quite different when compared to most of
the previous findings [15],[47],[49] which found that the increase of %LOI of fly ash
results in low compressive strength.
Ref. code: 25605722040416SAT
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Figure 6.1 Compressive strength of fly ash concrete containing various %LOI
(controlled slump by adjustment of water)
Figure 6.2 Compressive strength of OPC and fly ash concrete containing various
%LOI (controlled slump concrete by using superplasticizer)
40 3835
4844
41
59
5250
64 6260
0
10
20
30
40
50
60
70
80
FM0 FM6 FM12
Com
pre
ssiv
e S
tren
gth
(M
Pa)
Mix ID
3 days 7 days 28 days 91 days
37
27
3033 32 31
53
4648 49 48 48
61
56 57 58 57 56
69 71 71 7169 68
0
10
20
30
40
50
60
70
80
W400PC W40FM0 W40FM6 W40FM12 W40FM18 W40FM25
Com
pre
ssiv
e S
tren
gth
(M
Pa)
Mix ID
3 7 28 91
Ref. code: 25605722040416SAT
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6.2.2 Controlled water to binder ratio
Compressive strength of high LOI fly ash was also tested in controlled water to
binder conditions at w/b ratios of 0.4 and 0.5 as shown in Figures 6.3 and 6.4,
respectively.
The results were similar to compressive strength of controlled slump by the use
of superplasticizer case. Compressive strength of fly ash concrete tends to increase
with the increase in %LOI of fly ash for both tested w/b ratios (0.4 and 0.5). Although
the compressive strength of fly ash concrete tends to decrease when %LOI of fly ash
is beyond 12%, The overall compressive strength of high LOI fly ash concrete are
comparable to the low LOI fly ash (LOI=0.77%). In fact, long-term compressive
strength of high LOI fly ash mixture, having %LOI of 12% for w/b ratio of 0.4, is
even higher than those of the low LOI fly ash and OPC mixtures.
Ref. code: 25605722040416SAT
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Figure 6.3 Compressive strength of OPC and fly ash concrete containing various
%LOI (20% fly ash replacement, controlled w/b at 0.4)
Figure 6.4 Compressive strength of OPC and fly ash concrete containing various
%LOI (20% fly ash replacement, controlled w/b at 0.5)
52
4042 44 44 44
54
47 4850
4745
62 62 62 6461 61
6668 69
7169
67
0
10
20
30
40
50
60
70
80
W40OPC W40FM0 W40FM6 W40FM12 W40FM18 W40FM25
Com
pre
ssiv
e S
tren
gth
(M
Pa)
Mix ID
3days 7days 28days 91days
31
26 26 27 2728
37
32 3234 35
37
4441 42
43 4341
5249 50 51 50 49
0
10
20
30
40
50
60
70
80
W50OPC W50FM0 W50FM6 W50FM12 W50FM18 W50FM25
Com
pre
ssiv
e S
tren
gth
(M
Pa)
Mix ID
3days 7days 28days 91days
Ref. code: 25605722040416SAT
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6.3 Effect of fly ash content on compressive strength of high LOI fly ash
concrete
This section presents the effect of high LOI fly ash on compressive strength of
concrete with different replacement percentages of fly ash at ages of 3, 7, 28 and 91
days. The effect of fly ash content was investigated for w/b of 0.4 and 0.5 as shown in
Figures 6.5 and 6.6, respectively. Cement was partially replaced with fly ash, with
%LOI ranges from 0.77% to 25.37% by weight, at 20% and 40%. All mixtures were
cured in water till the test ages. Compressive strength of fly ash concrete tends to
increase when LOI increase up to about 12%. Decreasing in compressive strength was
found when the LOI of fly ash is beyond 12%. However, compressive strength of
mixtures with %LOI of 6%, 12%, 18% and 25% are nearly the same as the mix with
the lowest %LOI, which is 0.77%. Mixture with the fly ash having %LOI of 12.37%
seems to have the highest compressive strength for every replacement percentage.
Ref. code: 25605722040416SAT
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a) 3 days b) 7 days
c) 28 days d) 91 days
Figure 6.5 Compressive strength of low and high LOI fly ash concrete
with various %replacement of 20 and 40% (w/b = 0.4)
OPC= 52
0
10
20
30
40
50
60
70
80
0 6 12 18 25
Co
mpre
ssiv
e S
tren
gth
(M
Pa)
LOI of fly ash, %
r 20 r 40
OPC=5
4
0
10
20
30
40
50
60
70
80
0 6 12 18 25
Co
mpre
ssiv
e S
tren
gth
(M
Pa)
LOI of fly ash, %
r 20 r 40
OPC=6
2
0
10
20
30
40
50
60
70
80
0 6 12 18 25
Co
mpre
ssiv
e S
tren
gth
(M
Pa)
LOI of fly ash, %
r 20 r 40
OPC=66
0
10
20
30
40
50
60
70
80
0 6 12 18 25
Co
mpre
ssiv
e S
tren
gth
(M
Pa)
LOI of fly ash, %
r 20 r 40
Ref. code: 25605722040416SAT
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a) 3 days b) 7 days
c) 28 days d) 91 days
Figure 6.6 Compressive strength of low and high LOI fly ash concrete
with various %replacement of 20 and 40% (w/b = 0.5)
OPC=3
1
0
10
20
30
40
50
60
70
80
0 6 12 18 25
Co
mpre
ssiv
e S
tren
gth
(M
Pa)
LOI of fly ash, %
r20 r40
OPC=3
7
0
10
20
30
40
50
60
70
80
0 6 12 18 25
Co
mpre
ssiv
e S
tren
gth
(M
Pa)
LOI of fly ash, %
r20 r40
OPC=4
4
0
10
20
30
40
50
60
70
80
0 6 12 18 25
Co
mpre
ssiv
e S
tren
gth
(M
Pa)
LOI of fly ash, %
r20 r40
OPC=5
2
0
10
20
30
40
50
60
70
80
0 6 12 18 25
Co
mpre
ssiv
e S
tren
gth
(M
Pa)
LOI of fly ash, %
r20 r40
Ref. code: 25605722040416SAT
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6.4 Effect of different curing conditions on compressive strength of high LOI fly
ash concrete
Two curing conditions, water-cured (WC) and air-cured (AC) conditions, were
used to evaluate the effect of high fly ash in different curing condition. Fly ash was
used to replace cement at 20% by weight. Compressive strength was tested at two
ages, which are 28 days and 91 days.
6.4.1 Controlled water to binder
In this section, compressive strength of concrete were tested in controlled w/b
at 0.4. Figures 6.7a and 6.7b illustrate the compressive strength of high LOI fly ash
concrete in different curing conditions at 28 and 91 days, respectively. The dotted line
represents compressive strength of OPC concrete in water-cured condition. As
expected air-cured concrete shows lower compressive strength comparing to water-
cured concrete for every LOI level of fly ash. For water-cured concrete, compressive
strength of all fly ash mixtures having various %LOI were comparable to that of OPC
mixture at 28 days, but then higher at 91 days. While the compressive strength of all
fly ash mixtures of air-cured concrete were lower than OPC mixture at both 28 and 91
days. However, the increases in compressive strength are found in both type of curing
conditions. When LOI increases from 0.77% up to 12.37%, compressive strength also
gradually increases. After that, the decreases in compressive strength is found when
LOI level of fly ash is beyond 12%.
a) 28 days b) 91 days
Fig 6.7 Compressive strength of low and high LOI fly ash concrete
in different curing conditions ( controlled w/b at 0.4)
OPC=6
2
50
55
60
65
70
0 6 12 18 25
Co
mpre
ssiv
e S
tren
gth
(M
Pa)
LOI of fly ash, %
W40 (WC) W40 (AC)
OPC=6
6
55
60
65
70
75
0 6 12 18 25
Co
mpre
ssiv
e S
tren
gth
(M
Pa)
LOI of fly ash, %
W40 (WC) W40 (AC)
Ref. code: 25605722040416SAT
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6.4.2 Controlled slump by using superplasticizer
The effect of high LOI fly ash on compressive strength of concrete in different
curing condition was also tested in the condition such that slump of concrete was
controlled at 8.5 ± 1 cm by the use of superplasticizer. As illustrated in Figures 6.8a
and 6.8b, the results show the same tendency as the controlled w/b ratio case. Air-
cured concrete shows lower compressive strength than the water-cured concrete. The
effect of curing type on compressive strength of fly ash concrete can be clearly seen at
91 days. Concrete with %LOI of 12% demonstrates the highest compressive strength
in both water-cured and air-cured conditions. It should be noted here that the tested
compressive strength of the controlled OPC mixture in this section are slightly
different from those in the section 6.4.1(controlled water to binder) because they were
separately prepared.
a) 28 days b) 91 days
Fig 6.8 Compressive strength of low and high LOI fly ash concrete
in different curing conditions (controlled slump by using superplasticizer)
OPC=6
1
50
55
60
65
70
0 6 12 18 25
Co
mpre
ssiv
e S
tren
gth
(M
Pa)
LOI of fly ash, %
WC AC
OPC=6
9
55
60
65
70
75
0 6 12 18 25
Co
mpre
ssiv
e S
tren
gth
(M
Pa)
LOI of fly ash, %
WC AC
Ref. code: 25605722040416SAT
81
6.5 Curing sensitivity of high LOI fly ash concrete on compressive strength
The curing sensitivity of high LOI fly ash concrete on compressive strength
was evaluated by using the curing sensitivity index (CSIfc′) which is the percentage
difference between compressive strength of concrete that is continuously water-cured
and that of the continuously air-cured concrete as shown in equation (6.1). The higher
curing sensitivity index means concrete is more sensitive to curing. Since concrete
with high w/b is more sensitive to curing because the water loss due to evaporation is
easier when compare to the low w/b mixture. Thus, only curing sensitivities of low
w/b mixtures, which are controlled water to binder ratio concrete (w/b =0.40) and
controlled slump concrete at 8.5 ± 1 cm by the use of superplasticizer, were
investigated.
%, CSIf′c =fc′(WC) − fc′(AC)
fc′(WC)× 100 (6.1)
where CSIf′c is curing sensitivity index for compressive strength(%). fc′(WC) and
fc′(AC) are compressive strength of water-cured and air-cured specimens, respectively
(MPa).
It can be seen from Figures 6.9 and 6.10 that at the age of 28 days, CSIf′c of fly
ash concrete decreases when the %LOI of fly ash increases from 0.77 to 12% but then
start to increase again when %LOI of fly ash is greater than 12%. While CSIf′c at 91
days, gradually decreases until %LOI of fly ash increases up to 18%. It was found that
fly ash with the lowest %LOI (LOI=0.77%) has the highest CSIfc′ at both 28 days and
91 days for both cases, controlled w/b ratio (Fig 6.9) and controlled slump concrete
(Fig 6.10). The lowest CSIf′c was obtained in the mixture containing fly ash with
%LOI of 12% for concrete at 28 days and 18% for concrete at 91 days.
It is a common known that the CSIf′c of fly ash concrete is higher than that
OPC concrete. A study by Kinaanath Hussain [64] found that fly ash increases the
sensitivity of curing due to its slow reaction and it needs water for the pozzolanic
reaction process at long-term age. Another reason is that the rate of evaporation of fly
ash concrete is higher than cement-only concrete so early water loss by evaporation in
Ref. code: 25605722040416SAT
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air-cured fly ash concrete results in less water inside the concrete for pozzolanic
reaction [65]. At low w/b there is not enough water inside concrete and porosity of the
concrete is low, thus it is difficult for external water to penetrate into the concrete.
The result in this study indicates that high LOI fly ash is capable of reducing the
CSIf′c of fly ash concrete by its potential of internal curing ability. However, it should
be noted that too high percentage of LOI of fly ash could adversely affect the CSIf′c of
fly ash concrete as well as its compressive strength. From the discussion above, the
increase in compressive strength of high LOI fly ash might also be due to this internal
curing effect.
Fig 6.9 Curing sensitivity of fly ash concrete containing various %LOI
for controlled w/b case (w/b= 0.4)
12.88
7.69 7.06
9.55 10.38
14.13
11.75 10.95
10.20 10.15
0
5
10
15
20
FM0 FM6 FM12 FM18 FM25
CS
I fc'
(%
)
MIX ID
28days 91days
Ref. code: 25605722040416SAT
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Fig 6.10 Curing sensitivity of fly ash concrete containing various %LOI
for controlled slump at 8.5 cm by using admixture case
6.6 Microstructure study of high LOI fly ash concrete
In this part, some microstructure investigations were carried out in order to
find out the possible reasons or evidences to explain the increase in compressive
strength of high LOI fly ash concrete.
6.6.1 Porosity of fly ash mortars and concrete with different %LOI
Porosity of mortar and concrete containing fly ashes with various %LOI were
measured in term of total volume of permeable voids according to ASTM C642. The
total volume of permeable voids of fly ash mortar and concrete specimens, having
various %LOI of 0.77, 6 and 12%, were tested at water to binder ratio of 0.25 and 0.4,
respectively. Test was carried out at the age of 3 days for mortar specimens and 28
days for concrete specimens. Results of volume of permeable voids of the mortar and
concrete specimens are shown as illustrated in Figures 6.11 and 6.12, respectively. It
was found that higher %LOI of fly ash tends to slightly increase the total volume of
permeable voids of mortar or concrete.
The increase in porosity of high LOI fly ash can be one of the reasons that
support the increase in carbonation depth and the reduction in chloride resistance of
high LOI fly ash concrete. However, the increase in porosity of high LOI fly ash
3.89
2.07 1.89 2.13
3.94
14.76
11.81
10.04 9.16
9.77
0
5
10
15
20
FM0 FM6 FM12 FM18 FM25
CS
I fc'
(%
)
MIX ID
28days 91days
Ref. code: 25605722040416SAT
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seems to conflict with the increase in compressive strength of high LOI fly ash
concrete.
Figure 6.11 Total volume of permeable voids in fly ash mortars
with different %LOI at the age of 3 days
Figure 6.12 Total volume of permeable voids in fly ash concrete
with different %LOI at the age of 28 days
16.35 16.59 16.68
0
2
4
6
8
10
12
14
16
18
20
FM0 FM6 FM12
Vo
lum
e o
f per
mea
ble
vo
id (
%)
Mix ID
11.34 11.44 11.59
0
2
4
6
8
10
12
14
FM0 FM6 FM12
Vo
lum
e o
f per
mea
ble
vo
id (
%)
Mix ID
Ref. code: 25605722040416SAT
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6.6.2 Microstructure examination of high LOI fly ash concrete by SEM
Use of lightweight aggregates (LWA), which are porous materials, can
improve the interfacial transition zone (ITZ) of concrete by the formation of a dense
ITZ and thus enhances the concrete strength. Lightweight aggregates have high
absorption which can subsequently release water to increase the hydration degree of
the paste around the aggregates, making the paste to develop a structure with low
porosity [76][77]. Wasserman & Bentur [67] also added that for lightweight
aggregates of equal strength, the aggregate of higher absorption would provide higher
strength concrete due to its denser ITZ. Moreover, a study by Lo et al [78], which
used the sintered lightweight aggregate manufactured from high-carbon fly ash, also
found that cement paste infiltrated into the high-carbon fly ash light-weight aggregate
shell (see Figure 6.13), which can provide effective mechanical interlocking between
the light-weight aggregate and the cement paste at the ITZ.
(a) BSEI showing the penetration of cement paste into the HCFA-LWA surface
(x200)
Ref. code: 25605722040416SAT
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(b) Typical view of the HCFA-LWA/cement paste ITZ (x2000) after loading
Figure 6.13 ITZ microstructure of High-carbon fly ash lightweight aggregate
concrete, Lo et al (2016)
Investigation on the microstructure of high LOI fly ash concrete specimen was
carried out using scanning electron microscope (SEM). SEM pictures of fly ash and
carbon particles in polished surface are shown in Figures 6.14 and 6.15. In the
pictures, fly ash particles are white grey sphere particles, while carbon particle are the
black particles. It can be observed from the Figures 6.14 and 6.15 that the cement
paste infiltrated into the rough surface and pores of the carbon particles. This result is
similar to the microstructure of concrete using lightweight aggregate discussed above.
Cement might react with the additional water, absorbed by the carbon particles,
resulting in better bonding between cement and carbon particles and therefore, might
be one reason to not reducing the compressive strength of high LOI fly ash concrete,
in addition to the strength enhancing effect of hardshell formation contributed by
internal curing, that will be proven in the next section.
Ref. code: 25605722040416SAT
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Figure 6.14 Typical view of paste around a particle of fly ash and carbon
Figure 6.15 ITZ microstructure of a carbon particle and cement paste
Project 1 6/9/2017 11:22:23 AM
Comment:
50µm Electron Image 1
FeFe
Fe K
S
Mg
Al
Si
Ca
Ca
O
K
C
0 2 4 6 8 10 12 14 16 18 20keVFull Scale 10124 cts Cursor: 0.000
Sum Spectrum
Spectrum processing : Peak possibly omitted : 4.501 keV
Processing option : All elements analyzed (Normalised)Number of iterations = 5
Standard :C CaCO3 1-Jun-1999 12:00 AMO SiO2 1-Jun-1999 12:00 AMMg MgO 1-Jun-1999 12:00 AMAl Al2O3 1-Jun-1999 12:00 AMSi SiO2 1-Jun-1999 12:00 AMS FeS2 1-Jun-1999 12:00 AMK MAD-10 Feldspar 1-Jun-1999 12:00 AMCa Wollastonite 1-Jun-1999 12:00 AMFe Fe 1-Jun-1999 12:00 AM
Elem... Weight% Atomic% C K 46.46 59.57O K 32.39 31.17Mg K 0.71 0.45Al K 1.69 0.96Si K 4.50 2.47S K 0.40 0.19K K 0.31 0.12Ca K 12.25 4.71Fe K 1.29 0.36
Totals 100.00
Ref. code: 25605722040416SAT
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6.6.3 Experiment on micro hardness
Vickers hardness test was performed in two concrete mixtures, which are
W40FM0 (containing fly ash having LOI of 0.77%) and W40 FM12 (containing fly
ash having LOI of 12.37%) at the age of 28 days. In this test the Vickers hardness was
not performed at the paste near to sand particles but near to the fly ash and carbon
particles. Moreover, the hardness values at different distances from the particles of fly
ash and carbon were also measured. It is quite difficult to measure the exact hardness
value around the carbon particles because fly ash particles were spreading all over the
surface of concrete and also near to carbon particles. Therefore, the tested points
around the carbon particles were selected by avoiding those fly ash particles. Also
measuring the hardness value of fly ash particles is a tough work, because the
majority of fly ash particles are very small, only the hardness values of fly ash
particles having large size can be measured.
For the mixture W40FM0, which contains 0.77% LOI fly ash, hardness values
around fly ash particles were recorded as shown in Table 6.1. For the mixtures
W40FM12, which contains 12% LOI fly ash, the hardness values around carbon and
fly ash particles were measured as listed in Tables 6.2 and 6.3, respectively. Figures
6.16 to 6.18 show the average hardness values and their tested locations around the
fly ash and carbon particles of mixtures W40FM0 and W40FM12.
The average hardness values near to carbon particles of W40FM12 mixture
were higher than those near to fly ash particles of both W40FM0 and W40FM12
mixtures. This result might be due to the water supplied from unburned carbon
particles, which causes additional hydration, producing shell like structure around the
carbon particles. The results of hardness values, measuring at different distances from
the particles of fly ash and carbon, demonstrate that the hardness values near to
carbon particles decreases as the distance from the carbon particles increases (see
Figure 6.17 comparing cases 5 and 5-1). On contrary, the hardness values near to fly
ash particles tend to increase as the distance from the fly ash particles increases (see
Figure 6.16 comparing cases 1 and 1-1, Figure 6.18 comparing cases 2 and 2-1). The
high hardness values near the carbon particles coincide with the hardness results of
bottom ash concrete studied by Hussain [64] which reports that the hardness values
near the bottom ash particles, which is a porous material, are higher than sand
particles due to the formation of a hard shell around its particles.
Ref. code: 25605722040416SAT
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Table 6.1 Hardness values near fly ash particles of W40FM0 mixture
Tested
Point No.
Vickers Hardness Value near particle
1 1-1 2 3 4 5
1 29.84 36.28 29.84 26.08 32.04 39.24
2 27.25 43.71 24.98 34.49 31.28 43.79
3 40.31 41.42 40.31 43.79 30.55 47.74
4 33.65 30.55 35.37 42.58 29.84 43.79
5 30.55 39.24 30.55 41.42 38.21 52.15
6 28.51 - 23.46 - 25.52 49.17
7 - - 27.87 - - 35.37
8 - - 49.17 - - -
9 - - 47.74 - - -
Avg 31.69 38.24 34.37 37.67 31.24 44.46
Figure 6.16 Average hardness values near to fly ash particles with their tested
locations of concrete containing fly ash with %LOI of 0.77%
Ref. code: 25605722040416SAT
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Table 6.2 Hardness values near carbon particles of W40FM12 mixture
Tested
Point No.
Vickers Hardness Value near particle
1 2 3 4 5 5-1
1 75.71 52.25 52.25 57.43 69.96 41.42
2 59.33 50.68 53.89 55.63 53.89 42.5
3 53.89 52.25 75.71 53.89 71.65 45.05
4 55.62 - 67.95 54.47 53.89 47.95
5 69.96 - - - 61.32 -
6 59.33 - - - - -
7 55.62 - - - - -
Avg 61.35 51.73 62.45 55.36 62.14 44.23
Figure 6.17 Average hardness values near to carbon particles and their tested
locations of concrete containing fly ash with %LOI of 12%
Ref. code: 25605722040416SAT
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Table 6.3 Hardness values near fly ash particles of W40FM12 mixture
Tested
Point No.
Vickers Hardness Value near particle
1 2 2-1 2-2
1 29.17 63.42 46.36 39.24
2 43.79 55.62 47.74 29.84
3 - 39.24 - 35.37
4 - 27.87 - 29.26
5 - 31.28 - -
6 - 27.87 - -
7 - 40.31 - -
8 - 29.84 - -
9 - 45.05 - -
10 - 47.74 - -
Avg 36.48 40.82 47.05 33.43
Figure 6.18 Average hardness values near to fly ash particles and their tested
locations of concrete containing fly ash with %LOI of 12%
Ref. code: 25605722040416SAT
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Chapter 7
Results of Durability of High LOI Fly Ash Concrete
7.1 Effect of high LOI fly ash on carbonation resistance
In this study, fly ashes with various %LOI were used to partially replace
cement at 20%, by weight. Carbonation depth of water-cured and air-cured concrete
specimens with water to binder ratios of 0.4 and 0.5 were measured. Specimens were
exposed in the accelerated carbonation environment for 28 and 56 days, respectively.
Figures 7.1 and 7.2 show the effect of high LOI fly ash on carbonation depth
of water-cured concrete, which were exposed for 28 and 56 days, respectively. At the
same water to binder ratio, it was found that carbonation depth of concrete gradually
increased along with the increase in %LOI of fly ash. The same tendencies were
obtained for both tested water to binder ratios of 0.4 and 0.5.
Using fly ash as a cement replacing material has been found to lower the
carbonation resistance of concrete due to the two main reasons: (1) fly ash delay the
hydration reaction and increase the porosity of concrete (2) the reduction in calcium
hydroxide(CH) by pozzolanic reaction of fly ash and by the reduced cement content.
Horiguchi et al [70], malami et al [72], and Sulapha et al [74] demonstrated a
significant relation between carbonation depth and porosity of concrete, in which
carbonation rate increased when the total pore volume increased. Roy et al [73] also
added that concrete having larger pores had higher carbonation rate than concrete that
had smaller pores. Therefore, in this case the higher carbonation depth of higher LOI
fly ash concrete might be the result of the higher total porosity of concrete.
As for the effect of curing, air-cured concrete exhibits higher carbonation
depth than the water-cured concrete (see Figures 7.2a and 7.2b), expressing the
inadequate curing of specimens in air-cured condition. The carbonation depths of air-
cured concrete increase along with the increase of %LOI of fly ash.
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(a) 28 days
(b) 56 days
Figure 7.1 Carbonation depth fly ash concrete containing various %LOI
at different exposure periods, (water-cured condition)
0
2
4
6
8
10
12
14
16
0 6 12 18 25
Car
bon
atio
n D
epth
(m
m)
LOI level, %
W40(WC)
W50(WC)
0
2
4
6
8
10
12
14
16
0 6 12 18 25
Car
bon
atio
n D
epth
(m
m)
LOI level, %
W40(WC)
W50(WC)
Ref. code: 25605722040416SAT
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(a) 28 days
(b) 56 days
Figure 7.2 Carbonation depth fly ash concrete containing various %LOI
at different exposure periods, (water-cured and air-cured conditions)
0
2
4
6
8
10
12
14
16
0 6 12 18 25
Car
bo
nat
ion D
epth
(m
m)
LOI level, %
W40(WC)
W50(WC)
W40(AC)
W50(AC)
0
2
4
6
8
10
12
14
16
0 6 12 18 25
Car
bon
atio
n D
epth
(m
m)
LOI level, %
W40(WC)
W50(WC)
W40(AC)
W50(AC)
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Curing sensitivity of high LOI fly ash concrete on carbonation at w/b of 0.4
was evaluated, in addition to the curing sensitivity based on compressive strength, by
using the curing sensitivity index ( CSICO2) which is the percentage difference
between carbonation depth of concrete that is water-cured and that of the air-cured
concrete as shown in equation (7.1). The higher curing sensitivity index means the
concrete is more sensitive to curing
%, CSICO2=
C𝑑(WC) − Cd(AC)
Cd(WC)× 100 (7.1)
where CSICO2is curing sensitivity index for carbonation (%). C𝑑(WC) and C𝑑(AC) are
carbonation depth of water-cured and air-cured specimens, respectively (mm).
Although the carbonation depth of concrete gradually increases with the
increase of %LOI of fly ash, high LOI fly ashes can reduce the curing sensitivity of
on carbonation (see Figure 7.3a). It can be seen that the CSICO2 based on carbonation
at 28 days of exposure had the similar tendency to that of CSIf𝑐′ based on compressive
strength (see Figures 6.9 and 6.10). The CSICO2 of fly ash concrete gradually
decreases from 49.46 to 35.65% when the %LOI of fly ash increases from 0.77%
(FM0) to 18.41% (FM18). Although the CSICO2 of fly ash having %LOI of
25.37%(FM25) starts to increase, Its CSICO2 is still lower than the fly ash with the
lowest LOI (LOI =0.77%). However, at longer exposure period, the ranges of %LOI
which allow high LOI fly ash concrete to perform better than low LOI fly ash were
smaller (see Figure 7.3b). In fact, fly ashes with LOI in the ranges of 0.77 to 18.41%
have similar CSICO2. A study by T.-H. Ha et al [14] demonstrated that the alkalinity of
fly ash mortar was greatly affected with the increase in carbon content, which may be
due to the reaction of carbon with the oxygen in the atmosphere thereby accelerating
the carbonation process. This might be another reason that the CSICO2of fly ash
concrete containing very high %LOI, which is generally known to contain with large
amount of unburned carbon particles, tends to greatly increase at longer exposure
period.
Ref. code: 25605722040416SAT
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(a) 28 days of exposure
(b) 56 days of exposure
Fig 7.3 Curing sensitivity index based on carbonation of fly ash concrete
containing various %LOI at different exposure periods, (w/b=0.4)
49.4645.59
38.2135.65
42.50
0
10
20
30
40
50
60
70
80
FM0 FM6 FM12 FM18 FM25
CS
I CO
2(%
)
MIX ID
43.7541.18
43.48 45.16
57.14
0
10
20
30
40
50
60
70
80
FM0 FM6 FM12 FM18 FM25
CS
I CO
2(%
)
MIX ID
Ref. code: 25605722040416SAT
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7.2 Effect of high LOI fly ash on chloride resistance
Chloride ion penetrability of OPC, low and high LOI fly ash concrete was
tested at water to binder ratios of 0.4 and 0.5. The charge passed results of OPC
mixture at 28, 56 and 91 days for water to binder ratio of 0.4 were 3945, 3366 and
3180, respectively and those for water to binder ratio of 0.5 were 7173, 6993 and
6879, respectively. Figures 7.4 and 7.5 show chloride ion penetrability of fly ash
concrete containing various %LOI at water to binder ratios of 0.4 and 0.5,
respectively. The overall results show that the charge passed values of fly ash
concrete with all %LOI level were lower than that of the OPC concrete at every tested
age. The lower chloride ion penetrability of concrete containing fly ash is related to
the refined pore structure and its reduced electrical conductivity [75]. However, when
comparing among the fly ash concrete, the charge passed values tend to increase with
the increase of %LOI of fly ash. The increase was smaller when the water to binder is
low (see Figure 7.4) but it could be clearly seen when w/b is high (see Figure 7.5).
The result indicates the poorer chloride resistance of higher %LOI fly ash mixtures
comparing to the lower LOI one. This result coincides with the total porosity results
in Chapter 6, which found that higher LOI of fly ash tends to increase total porosity of
the mortar and concrete, which therefore in this case lowers the chloride penetration
resistance of concrete. A study by T.-H. Ha et al [14] also found that the increase in
activated carbon content accelerated the corrosion of rebars in mortar containing fly
ash with different percentages of carbon.
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Figure 7.4 Chloride permissibility of fly ash concrete containing various %LOI
by measuring charge passed (w/b = 0.4)
Figure 7.5 Chloride permissibility of fly ash concrete containing various %LOI
by measuring charge passed (w/b = 0.5)
OPC 91 days
OPC 56 days
OPC 28 days
0
1000
2000
3000
4000
5000
6000
7000
8000
0 6 12 18 25
Char
ge
pas
s (c
oulo
mb
)
LOI of fly ash, %
28d
56d
91d
OPC 28 days
OPC 56 days
OPC 91 days
OPC 91 daysOPC 56 days
OPC 28 days
0
1000
2000
3000
4000
5000
6000
7000
8000
0 6 12 18 25
Char
ge
pas
s (c
oulo
mb
)
LOI of fly ash, %
28d
56d
91d
OPC 28 days
OPC 56 days
OPC 91 days
Ref. code: 25605722040416SAT
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7.3 Effect of high LOI fly ash on shrinkage
7.3.1 Autogenous shrinkage
Test results of autogenous shrinkage of paste specimens with water to binder
ratios of 0.25 and 0.40 are shown in Figures 7.6 and 7.7 respectively. It was found
that the use of fly ash with %LOI, ranging from 0.77 to 25%, reduces autogenous
shrinkage of concrete significantly comparing to the OPC concrete. Moreover, fly ash
with higher %LOI was even more effective to reduce the autogenous shrinkage than
the fly ash with low %LOI. This proves the internal curing ability of high LOI fly ash,
which is a porous material. A study by Hussain [64] found that the use of bottom ash,
which is also a porous material, significantly reduced autogenous shrinkage of
mortars and concrete due to its internal curing ability.
Figure 7.6 Autogenous shrinkage of pastes containing fly ashes with various %LOI
(w/b = 0.25)
-1000
-800
-600
-400
-200
0
0 4 8 12 21 35 49 63 77 91
Auto
gen
ous
shri
nkag
e (m
icro
n)
Age (days)
OPC FM0 FM6 FM12 FM18
Ref. code: 25605722040416SAT
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Figure 7.7 Autogenous shrinkage of pastes containing fly ashes with various %LOI
(w/b = 0.4)
7.3.2 Total shrinkage
The effect of high LOI fly ashes on total shrinkage is shown in Figures 7.8 and
7.9. It can be seen from these Figures that shrinkage of higher %LOI fly ash mixture
is higher than the mixtures that incorporate lower %LOI fly ash in both tested w/b of
0.4 and 0.5. The total shrinkage of paste gradually increases with the increase of
%LOI of fly ash. However, the use of fly ash with various %LOI (LOI=0.77 to 25%)
can reduce the total shrinkage when compared to the OPC mixture, since their total
shrinkages are still lower than that of the OPC mixture. But, it should be noted that fly
ash with very high %LOI could further increase the total shrinkage since it increase
the porosity of the concrete.
-1000
-800
-600
-400
-200
0
0 4 8 12 21 35 49 63 77 91A
uto
gen
ous
shri
nkag
e (m
icro
n)
Age (days)
OPC FM0 FM6 FM12 FM18
Ref. code: 25605722040416SAT
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Figure 7.8 Total shrinkage of pastes containing fly ashes with various %LOI,
(w/b = 0.25)
Figure 7.9 Total shrinkage of pastes containing fly ashes with various %LOI,
(w/b = 0.4)
-2500
-2000
-1500
-1000
-500
0
0 4 8 12 21 35 49 63 77 91T
ota
l sh
rinkag
e (m
icro
n)
Age (days)
OPC FM0 FM6 FM12 FM18
-2500
-2000
-1500
-1000
-500
0
0 4 8 12 21 35 49 63 77 91
To
tal sh
rinkag
e (m
icro
n)
Age (days)
OPC FM0 FM6 FM12 FM18
Ref. code: 25605722040416SAT
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Chapter 8
Conclusions and Recommendations
8.1 Conclusions
This study examined the effects of high LOI fly ash on workability, compressive
strength and some durability properties of concrete by using artificial high LOI fly
ashes having various %LOI ranges from 0.77 to 25%. Based on all of the
experimental results in this study, the performances of high LOI fly ash mixtures
compared to low LOI fly ash mixtures having %LOI of 0.77% and cement-only
mixture are summarized and shown in Table 8.1 and Table 8.2, respectively.
Table 8.1 Performances of high LOI fly ash compared with low LOI fly ash
Test item Better Similar Worse
Workability
Water requirement
Initial slump
Compressive strength
Early compressive strength*
Long-term compressive strength*
Durability
Autogenous shrinkage
Total shrinkage**
Carbonation resistance
Chloride resistance (RCPT)**
Remark: *Better or similar depends on the level of %LOI of fly ash, the worse case
were only found in the case of controlled slump by adjustment of water.
**Performances are still better than those of cement-only mixtures.
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Table 8.2 Performances of high LOI fly ash mixture compared with cement-only
mixture
Test item Better Similar Worse
Workability
Water requirement*
Initial slump*
Compressive strength
Early compressive strength
Long-term compressive strength*
Durability
Autogenous shrinkage
Total shrinkage*
Carbonation resistance
Chloride resistance (RCPT)
Remark: *Better or similar or worse depends on the level of %LOI of fly ash
Apart from the performances of high LOI fly ash shown in Tables 8.1 and 8.2,
the results in the other aspects are additionally concluded as follows:
1. The moisture content of fly ash increases with the increase of its %LOI.
However, the moisture content of fly ash having %LOI of 25% is still lower than
the limit in ASTM standard specification, which limits the maximum moisture
content of fly ash used in concrete at 3%.
2. Particle size distributions of the prepared high LOI fly ashes are coarser than the
low LOI fly ash, whereas the Blaine fineness of high LOI fly ashes are higher.
This proves that high LOI fly ashes used in this study really have more porous
structure and contain irregular particles, because of the added PAC particles.
3. Water retainability of fly ash increases when %LOI of fly ash increases due to the
porous and rough-texture particles of the added PAC. Therefore, high LOI fly
ashes increase the water requirement of the mixtures.
4. Using low LOI fly ash significantly improves the slump of concrete compared to
the cement-only mixture. However, slump of fly ash concrete was significantly
affected by the %LOI of fly ash. The initial slump of concrete gradually
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decreases with the increase of %LOI of fly ash. Nevertheless, using fly ash
having %LOI of 0.77% to 6% with replacement percentage of 20% in the mixture
seems to improve the workability of concrete comparing to the cement-only
mixture.
5. Increase percent replacement of fly ash from 20% to 40% significantly enhances
slump of fly ash concrete having %LOI of 0 to 12%. On the contrary, the slump
of concrete with 40% fly ash replacement gradually decreases and becomes
worse than that of 20% replacement when %LOI of fly ash is over 12%. This
phenomenon is because when the high amount of fly ash, having very high %LOI
is used in the mixture, its water retainability plays the more important role than
its lubrication effect.
6. The reduction in compressive strength of high LOI fly ash concrete was obtained
in the case of the controlled slump by adjustment of water. However, the increase
in compressive strength of high LOI fly ash concrete was obtained in the cases of
the controlled slump by the use of superplasticizer and controlled w/b. In these 2
cases, the compressive strength of concrete gradually increases when %LOI of
fly ash increase from 0 to 12%. Although the compressive strength tends to
gradually decrease when %LOI of fly ash is beyond 12%, the overall
compressive strength of high LOI fly ash concrete is comparable to fly ash
concrete with the lowest %LOI (LOI=0.77%).
7. Increase the replacement percentage of fly ash from 20% to 40% resulted in
lower compressive strength for fly ash with all %LOI.
8. Using high LOI fly ashes in the mixtures can reduce the curing sensitivity of fly
ash concrete, especially the one that containing %LOI of 12% due to its internal
curing effect.
9. Although high LOI fly ashes increase porosity of concrete, the increase in
compressive strength of high LOI fly ash concrete was found to be due to its
internal curing effect. SEM pictures of polished high LOI fly ash concrete
showed that cement paste infiltrated into the rough surface and pores of the
carbon particles. Cement and fly ash might react with the additional water,
absorbed by the carbon particles, resulting in better bonding between cement and
carbon particles. Moreover, the result from micro hardness test of high LOI fly
ash concrete also revealed that the hardness values near to carbon particles were
Ref. code: 25605722040416SAT
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higher than those near to fly ash particles, proofing the existence of hard shell
around the carbon particles.
10. Carbonation and chloride resistance of high LOI fly ash concrete is worse than
the low LOI fly ash concrete. However, the effect of LOI of fly ash was less
significant when using in low w/b concrete.
11. Autogenous shrinkage of high LOI fly ash was significantly decreased. This
result is one of the evidences indicating the internal curinag ability of high LOI
fly ash.
12. Total shrinakge of high LOI fly ash was gradually increased with the increase of
%LOI of fly ash. However, the use of fly ash with %LOI of 0.77 to 25% can
reduce the total shrinkage when compared to the OPC mixture.
8.2 Recommendations for future studies
1. In this current study, the effect of high LOI fly ash has been carried out, by using
artificial high LOI fly ash produced from Mae-Moh fly ash. Mae-Moh fly ash is
low LOI fly ash but high in CaO content, which might be one of the reasons for
the strength gains of high LOI fly ash in this study. Therefore, the performances
of artificial high LOI fly ash produced from low CaO fly ash should be further
investigated.
2. The comparison between performances of artificial high LOI and real high LOI
fly ash should be further investigated.
Ref. code: 25605722040416SAT
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Appendices
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Appendix A
Physical properties of fine and coarse aggregates
Table A1 Physical properties of fine and coarse aggregates used in this study
Properties Fine aggregate Coarse aggregate
Bulk specific gravity (SSD) 2.59 2.83
Absorption (%) 1.16 0.34
Specific surface area, Ss (cm2/kg) 23429 1847
S/A minimum void (by volume) 0.43
Minimum void (%) 23.80
Fig A1 Sieve analysis result of fine aggregate
0
20
40
60
80
100
120
0.01 0.10 1.00 10.00 100.00
Cum
ula
tive
pas
sing (
%)
Sieve Size (mm)
Coarse limit fine limit River sand
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Fig B2 Sieve analysis result of coarse aggregate
0
10
20
30
40
50
60
70
80
90
100
1 10 100
% P
assi
ng
Sieve Size (mm)
Coarse limit Fine limit Crushed limestone
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Appendix B
An example of mix proportion calculation for making
artificial high LOI fly ashes
Table B.1 Chemical compositions of Mae-Moh fly ash and PAC-BC
Powder Loss on Ignition, %
Mae-Moh fly ash 0.77
PAC-BC 86.18
For example:
Need 20kg of artificial high LOI fly ash having %LOI of 18% (FM18).
%replacement of PAC = 18% − 0.77% = 17.23%
WPAC-BC = 20 kg × 17.23% = 3.446 kg
WFA = 20 kg – 3.446 kg = 16.554 kg
WPAC’-BC = 3.446 kg / 86.18% = 3.999 kg
Therefore, the mix proportion for FM18 is:
Mae-Moh fly ash = 16.554 kg
PAC-BC = 3.999 kg
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